795 KFT Titrino - Login
Transkript
795 KFT Titrino - Login
CH-9101 Herisau/Switzerland E-Mail [email protected] Internet www.metrohm.com 795 KFT Titrino Program version 5.795.0010 Instructions for Use 8.795.1003 11.2001 / pkl Table of contents Table of contents 1 Introduction ................................................................................................................ 1 1.1 Instrument description ................................................................................................ 1 1.2 Controls and parts ...................................................................................................... 2 2 Manual operation ....................................................................................................... 6 2.1 Keypad........................................................................................................................ 6 2.2 Principle of data input ................................................................................................. 7 2.3 Text input .................................................................................................................... 8 2.4 Configuration, key <CONFIG>.................................................................................. 9 2.5 Key <MODE> .......................................................................................................... 14 2.6 Parameters, key <PARAM>..................................................................................... 15 2.6.1 Parameters for KFT ............................................................................................ 15 2.7 Result calculations.................................................................................................... 25 2.8 Statistics calculation ................................................................................................. 28 2.9 Common variables.................................................................................................... 30 2.10 Data output ............................................................................................................. 31 2.10.1 Reports for the output at the end of a determination....................................... 31 2.10.2 Display of the Curve......................................................................................... 33 2.11 User name, key <USER> ...................................................................................... 34 2.12 Method memory key <USER METH> ................................................................... 35 2.13 Current sample data, key <SMPL DATA>............................................................. 37 2.14 Silo memory for sample data.................................................................................. 38 2.15 Storing determination results and silo calculations ................................................ 41 2.15.1 Storing determination results ........................................................................... 41 2.15.2 Silo calculations ............................................................................................... 42 2.16 Manual dosing ........................................................................................................ 44 3 Operation via RS232 Interface ................................................................................ 45 3.1 General rules............................................................................................................. 45 3.1.1 Call up of objects ............................................................................................... 46 3.1.2 Triggers .............................................................................................................. 47 3.1.3 Status messages ............................................................................................... 48 3.1.4 Error messages.................................................................................................. 49 3.2 Remote control commands ...................................................................................... 52 3.2.1 Overview............................................................................................................. 52 3.2.2 Description of the remote control commands ................................................... 67 3.3 Properties of the RS 232 Interface ............................................................................ 90 3.3.1 Handshake......................................................................................................... 90 3.3.2 Pin Assignment .................................................................................................. 93 3.3.3 What can you do if the data transfer does not work? ........................................ 95 4 Error messages and Troubleshooting ................................................................... 97 4.1 Error and special messages ..................................................................................... 97 4.2 Diagnosis ................................................................................................................ 100 4.2.1 General............................................................................................................. 100 4.2.2 Procedure......................................................................................................... 100 4.2.3 Equipment required: ........................................................................................ 101 4.2.4 Diagnosis steps ............................................................................................... 101 795 KFT Titrino Table of contents 4.3 Initialize and test RAM ............................................................................................ 110 4.4 Releasing a locked spindle .................................................................................... 111 5 Preparations ...........................................................................................................112 5.1 Setting up and connecting the instruments ........................................................... 112 5.1.1 Titrino with Stirrer or Titration Stand................................................................. 112 5.1.2 Connection of a printer .................................................................................... 113 5.1.3 Connection of a balance.................................................................................. 114 5.1.4 Connection of a KF Oven ................................................................................ 115 5.1.5 Connection of a Sample Changer ................................................................... 116 5.1.6 Connection of the 774 Oven Sample Processor ............................................. 117 5.1.7 Connection of a computer ............................................................................... 118 5.1.8 Connection of a Remote Box........................................................................... 118 5.2 Connection of electrodes and preparing titration vessel........................................ 122 6 Appendix .................................................................................................................123 6.1 Technical specifications ......................................................................................... 123 6.2 Pin assignment of the "Remote" socket.................................................................. 125 6.2.1 Lines of the "Remote" socket during the titration ............................................. 127 6.2.2 Possible configurations of the activate pulse KFT........................................... 128 6.3 User methods ......................................................................................................... 129 6.3.1 General ............................................................................................................ 129 6.3.2 KF Titer determination with H2O or methanol standard "H2OTiter" ................. 130 6.3.3 KF Titer determination with sodium tartrate "TarTiter"...................................... 131 6.3.4 Blank determination for KFT "Blank_KF".......................................................... 132 6.3.5 KF-titration with blank value subtraction "KF-Blank" ........................................ 133 6.3.6 KF-titration without blank value subtraction "KF" ............................................. 135 6.3.7 KF titrations with various KF reagents ............................................................. 137 6.3.8Determination of the bromine number "BrNumber" .......................................... 138 6.4 Titrino validation...................................................................................................... 139 6.4.1 Electronic tests ................................................................................................ 139 6.4.2 Wet tests .......................................................................................................... 139 6.4.3 Maintenance and adjustment of the Titrino ..................................................... 139 6.5 Warranty and conformity ........................................................................................ 140 6.5.1 Warranty........................................................................................................... 140 6.5.2 EU Declaration of conformity........................................................................... 141 6.5.3 Certificate of Conformity and System Validation ............................................. 142 6.6 Scope of delivery and ordering designations......................................................... 143 Index ...........................................................................................................................147 795 KFT Titrino Introduction 1 Introduction 1.1 Instrument description The 795 KFT Titrino is a fast and precise Titrator for the water determination according to Karl Fischer. The 795 KFT Titrino is equipped with a LCD graphical display on which titration curves can be observed in real-time. Ready-to-start methods for the most common applications are stored in the internal method memory. The operator is free to modify and overwrite this methods or to create and store his own titration sequences. Data exchange with a PC is possible with the Metrodata VESUV Software and with Metrodata TiNet Software complete remote control, data acquisition and evaluation via PC is enabled. 795 KFT Titrino 1 Introduction 1.2 Controls and parts Front view of instrument: 2 795 KFT Titrino Introduction 1 Exchange Unit 2 Display 3 Setting of display contrast 4 Controls the dosing rate during manual dosing with <DOS> and subsequent filling 5 Control keys and indicator lamps on the Titrino Key < > Power switch Key < > Switching stirrer ON/OFF Key <DOS> Dosing key. Dispensing is performed as long as <DOS> is being pressed. Used e.g. to prepare the Exchange Unit. The dispensing rate can be set with potentiometer (5). Key <STOP/FILL> - Stops procedures, e.g. titrations, conditioning. - Filling after manual dosing with <DOS>. Key <START> Starts procedures, e.g. titrations, conditioning. Identical with key <START> of the separate keypad. Indicator lamps: "COND." Lamp flashes when conditioning is performed and the titration vessel is still wet. It is on if conditioning is ok. "STATISTICS" Lamp is on when the "statistics" function (calculation of mean and standard deviation) is on. "SILO" Lamp is on when silo memory (for sample data) is on. 795 KFT Titrino 3 Introduction Rear view of instrument: 4 795 KFT Titrino Introduction 6 RS232 interfaces 2 separate interfaces for the connection of printer, balance, and computer 7 Remote lines (input/output) for the connection of the Remote Box, Sample Changers, robots etc. 8 Connection of electrodes • 1 measuring input for polarized electrodes, e.g. KF electrode 9 Connection for separate keypad 10 Connection for power cable With power supplies where the voltage is subject to severe HF disturbances, the Titrino should be operated via an additional power filter, e.g. Metrohm 615 model. 11 Connection for stirrer 728 Magnetic Stirrer, 802 Rod Stirrer, 703 or 727 Ti Stand Supply voltage: 10 VDC (I ≤ 200 mA) 12 Rating plate with fabrication, series and instrument number 795 KFT Titrino 5 2.1 Keypad 2 Manual operation 2.1 Keypad CONFIG Configuration. PARAM Parameters. SMPL DATA Sample data. STATISTICS ON/OFF switching of statistics calculations of consecutive determination, see page 28. MEAS/HOLD ON/OFF switching of measurements between titrations and hold during titrations. SILO ON/OFF switching of silo memory for sample data, see page 38. C-FMLA Calculation values, see page 27. DEF Formulas, data output, see page 25ff. USER METH Management of internal method memory, see page 35. PRINT Printing of reports, see page 33. REPORTS Result output. MODE Mode dialogue, see page 14. USER User name, see page 34. CURVE Switching result/curve display, see page 33. ←,→ Selection of special values (dialog marked with ":"). ↑,↓ Cursor key for navigation. CLEAR Clears values, set special values. ENTER Stores values. STOP Stops methods. QUIT Quits inquiries, waiting times, printing. START Starts methods. The third functions (inscriptions in the triangle) on the keys of the keypad are used for formula entry, see page 25. 6 795 KFT Titrino 2.2 Principle of data input 2.2 Principle of data input configuration >monitoring >peripheral units >auxiliaries >RS232 settings COM1 >RS232 settings COM2 >common variables configuration >peripheral units send to COM1: IBM send to COM2: IBM man.reports to COM: 1 balance: Sartorius stirrer control: OFF remote box: OFF • If you press a key, you will find a group of inquiries in the display. Example key <CONFIG>: In the first line you see where you are: You pressed key <CONFIG> and you are now in the inquiries "configuration". • The cursor is inverted. In our example the cursor is on the inquiry ">monitoring". You can move the cursor up and down with keys <↑> and <↓>. • If a dialog text is marked with ">", it contains a group of inquiries itself. You go to this group pressing <ENTER>. Example inquiries of "peripheral units": The first two lines indicate again where you are. Then you find the inquiries. If a dialog text of an inquiry is marked with ":", you can select a value with keys <←> and <→> (forward/backward). • A value is stored with <ENTER> and the cursor moves to the next inquiry. configuration >monitoring >peripheral units >auxiliaries >RS232 settings COM1 >RS232 settings COM2 >common variables 795 KFT Titrino • With key <QUIT> you move one level up, in our example you go back to ">peripheral units". If you press <QUIT> once more, you quit the inquiries in "configuration" altogether. • If you can scroll, "↓" or "↑" appear in the right lower or upper corner of the display. 7 2.3 Text input 2.3 Text input Example storing a method: user methods >store method method name: ******** • Delete this name with <CLEAR>. <CLEAR> REPORTS . ABC user methods >store method: method name: ABCDEFGHIJKLMNOPQRSTUVWXYZ abcdefghijklmnopqrstuvwxyz µ°!"#$&'()*+,-./ 0123456789 <QUIT> user methods >store method method name: <ENTER> 8 • Press key <USER METH>. Place the cursor to ">store method" and press <ENTER>. The name of the method which is currently in the working memory is displayed. Text • Open the "text writing mode" with key <ABC>. You can now select the desired character by means of the cursor keys, then confirm this character. Select the next character... When you confirmed the last character, i.e. your name is complete, you quit the text writing mode with <QUIT>. Confirm now the name with <ENTER>. • During text input you can correct typing errors with <CLEAR>: <CLEAR> deletes the characters one by one. • If you wish to modify an existing name, do not delete the existing name before you start the text input mode. Proceed then as follows: 1. Press <USER METH>, place the cursor to ">store method" and press <ENTER>. 2. Open the text writing mode directly: Press key <ABC>. 3. <CLEAR> now deletes the characters one by one or you can add additional characters. 4. If your text is complete, leave the text writing mode with <QUIT> and confirm the text with <ENTER>. 795 KFT Titrino 2.4 Configuration, key <CONFIG> 2.4 Configuration, key <CONFIG> Key <CONFIG> serves to enter device specific data. The set values apply to all modes. monitoring: Monitoring of instrument validation, service interval and printout of diagnostic report. peripheral units: Selection of printer, balance, stirrer control and COM for manual report output. auxiliaries: e.g. setting of dialog language, date, time, type of result display. RS232 settings COM1 and 2: RS parameters for the COM's. common variables: Values of common variables. CONFIG configuration >monitoring >peripheral units >auxiliaries >RS232 settings COM1 >RS232 settings COM2 >common variables The display texts of the Titrino are shown on the left side. The values are the default values. Monitoring functions >monitoring validation: time interval time counter service: next service 795 KFT Titrino OFF 365 d 0 d OFF YYYY-MM-DD Monitoring the validation interval (ON, OFF) Monitoring is carried out at the end of the titrations and when the Titrino is switched on. If the monitoring responds the message "validate instrument" appears. The message vanishes with <CLEAR>. At the same time the counter is reset to zero. If "ON" has been set: Time interval for validation (1...9999 d) see also page 139. Time counter (0...9999 d) Counts the number of days since the last time the counter was reset. Monitoring the service interval (ON, OFF) Monitoring is carried out after the Titrino has been switched on. If the monitoring responds the message "Service is due" appears. The message vanishes with <CLEAR>. If "ON" has been set: Date of next service (YYYY-MM-DD) 9 2.4 Configuration, key <CONFIG> system test report: OFF Settings for peripheral units >peripheral units send to COM1: IBM send to COM2: IBM man.reports to COM: balance: 1 Sartorius Selection of printer (Epson, Seiko, Citizen, HP, IBM) at the Titrino COM1 "Epson", for Epson "Seiko", e.g. for DPU-414 "Citizen", e.g. for iDP 562 RS, Custom DP40-S4N "HP" e.g. for Desk Jet types. Place curves always at the beginning of a page as you cannot have them over 2 pages. "IBM" for all printers with IBM character set Table 437 and IBM graphics, as well as for the data transmission to a computer or a data system. COM of Titrino for the output of manually triggered reports (1, 2, 1&2) Manually triggered reports (e.g. with <PRINT> ....). Exception <PRINT><REPORTS>: These reports are outputted on the COM as defined in the method. Selection of balance (Sartorius, Mettler, Mettler AT, AND, Precisa) Sartorius: Models MP8, MC1 Mettler: Models AM, PM, AX, MX, UMX and balances with 011, 012, and 016 interfaces Mettler AT: Model AT AND: Models ER-60, 120, 180, 182, FR-200, 300 and FX-200, 300, 320 Precisa: Models with RS232C interface stirrer control: OFF Automatic switching ON/OFF of the stirrer in the titration sequence (ON, OFF) If stirrer control is ON, the stirrer will be switched on at the beginning and switched OFF at the end of a determination. For KFT with conditioning the stirrer will be switched off in the inactive state. For stirrer control the red switch on the stirrer unit must be ON. remote box: OFF Connection of a remote box (ON ,OFF) To the remote socket for PC keyboard and barcode reader, see page 118. keyboard: 10 System test report printout (ON, OFF) With "ON" the report of the system test is printed out after the Titrino has been switched on, see also page 139. US If "ON" has been set: Type of PC keyboard (US, German, French, Spanish, Swiss.) The PC keyboard is used as an input aid, see page 119. 795 KFT Titrino 2.4 Configuration, key <CONFIG> barcode: input Target for barcode reader (input, method, id1, id2, id3, smpl size) The barcode reader is used as an input aid, see page 118. Input: The barcode string goes to the entry field in which the cursor is currently located. Method: The barcode string goes to the entry field "Methods" in the silo memory. Id1: The barcode string goes to the entry field "Id1". (Similar for Id2 and Id3.) Smpl size: The barcode string goes to the entry field "smpl size". General settings >auxiliaries dialog: english date 2001-11-15 time 08:13 Selection of dialog language (english, deutsch, français, español, italiano, portugese, svenska) Current date (YYYY-MM-DD) Format: Year-month-day, entry with leading zeros. Current time (hh-mm) Format: Hours-minutes, entry with leading zeros. Current run number for result output (0...9999) The sample number is set to 0 when the instrument is switched on and incremented on every determination. run number 0 auto start OFF Automatic start of titrations. (1...9999, OFF) Number of automatic starts ("number of samples"). Used for instrument interconnections in which the external instrument does not initiate a start. Not advisable in connections with Sample Changers. start delay 0 s Start delay (0...999999 s) Delay time after start of methods. Abort start delay time with <QUIT>. result display: bold Individual identification of devices (up to 8 ASCII characters) Will be printed in the result report, see page 32. dev.label. program 795 KFT Titrino Type of result display at the end of the determination (bold, standard) bold: The calculated results are displayed in bold characters. standard: Displays the whole information, e.g. results, endpoints, messages etc. 795.0010 Display of program version 11 2.4 Configuration, key <CONFIG> Settings of RS232 interface see also page 90 Identical for COM2. >RS232 settings COM1 baud rate: 9600 Baud rate (300, 600, 1200, 2400, 4800, 9600, 19200, 38400, 57600, 115200) data bit: 8 Data bit (7, 8) stop bit: 1 Stop bit (1, 2) parity: handshake: none HWs Handshake (HWs, SWline, SWchar, none) see page 90. Values of the common variables >common variables C30 Parity (even, odd, none) 0.0 etc. Common variables C30...C39 (0.. ± 999999) The values of all common variables are displayed. For creating common variables see page 30. Settings with key <CONFIG> and power ON Proceed as follows: 1. Switch the Titrino OFF. 2. Press <CONFIG> and keep it pressed during switching the Titrino ON. The display shows the following: 12 Setup >lock >curve lock: Locking keys <CONFIG>, <PARAM> and <SMPL DATA>, and the functions "recall method", "store method" and "delete method" of the internal method memory in the Titrino. curve: Changes the appearance of the curve printout. >lock lock "ON" means that the corresponding function is not accessible anymore. <configuration>: OFF <parameters>: OFF <smpl data>: OFF recall method: OFF store method: OFF delete method: OFF The corresponding key is locked. The corresponding function in the internal method memory of the Titrino is locked. 795 KFT Titrino 2.4 Configuration, key <CONFIG> curve The settings are valid for COM1 and COM2. If you change the printer type, the following settings are initialized according to the printer. >curve grid: ON Grid drawing (ON, OFF) frame: ON Frame drawing (ON, OFF) scaling: width length 795 KFT Titrino Full Type of scaling (Full, Auto) Full: The scaling goes from the greatest to the smallest value. auto: The scaling from tick to tick, e.g. the smallest/greatest values lie in between the first/last tick. 0.5 Width (0.2...1.00) 1 is greatest width. If you set 1, you may loose the label at the right margin. 0.05 Length (0.01...1.00) Time axis: Curve length 0.01 100 cm 0.1 10 cm 0.5 2 cm 1 1 cm 13 2.5 Key <MODE> 2.5 Key <MODE> MODE – With the key <MODE> the dialogue „mode“ is opened. ; mode mode: measured quantity: KFT Ipol The 795 Titrino is a titrator, specially designed for Karl Fischer water determinations. It has exclusively the mode KFT (Karl Fischer Titration). With <ENTER> the selection of the measured quantity is activated. Select Ipol or Upol with <←> or <→> and confirm it also with <enter>. The following modes can be selected: • KFT: Karl Fischer Titration, the determination of water content. The mode KFT is equipped with a set of standard parameters. They only need few settings in order to be ready to work. 14 795 KFT Titrino 2.6 Parameters, key <PARAM> 2.6 Parameters, key <PARAM> The key <PARAM> is used for the entry of values that determine the modes. Values marked with "cond." are accessible during the conditioning in the KFT mode. "**titr." means that these values can be changed during the titration. They influence the ongoing determination. Other values can only be changed in the inactive state. The display texts of the Titrino are shown on the left side. The values are the default values. PARAM 2.6.1 Parameters for KFT parameters >control parameters >titration parameters >stop conditions >statistics >preselections control parameters: for the EP. titration parameters control the general course of the titration. stop conditions: Parameters for the termination of the titration. statistics: Calculation of mean values and standard deviation, see page 28. preselections: ON/OFF of various auxiliary functions such as automatic requests after the start and activate pulse. >control parameters Control parameters EP at U 250 mV Endpoint (input range depending on the measured quantity: U, Ipol: 0.. ±2000 mV I, Upol: 0...±200.0 µA) 100 mV Control (input range depends on the measured quantity: U, Ipol: 1...2000 mV I, Upol: 0.1...200.0 µA) Outside of the control range: constant dosing, see page 21. cond. dynamics **titr. 795 KFT Titrino 15 2.6 Parameters, key <PARAM> max.rate max. ml/min **titr. min.volume incr. min. µl **titr. stop crit: drift **titr. stop drift 20 µl/min **titr. t(delay) 10 s **titr. stop time OFF s **titr. pause 1 **titr. 16 Minimum volume increment (0.1...9.9 µL, min.) <CLEAR> sets "min.". This parameter determines the addition rate at the start and the end of the titration, see also page 21. This parameter influences the titration speed and therefore its accuracy very strongly: A smaller "min.volume incr." results in a slower titration. Type of stop criteria (drift, time) Titration stops, if EP and stop drift are reached (1...999 µL/min) Titration stops if there is no dosing during t(delay) (0...999 s, INF) <CLEAR> sets "INF". Switch off when EP is reached and the set time after the last dosing has elapsed. If t(delay) is "INF" Stop after a time (0...999999 s, OFF) <CLEAR> sets "OFF". Stop after the set time after start of titration. "OFF" means no stop, i.e. titration for an "infinitely" long time. Titration parameters >titration parameters titr.direction: Maximum dosing rate (0.01...150 mL/min, max.) <CLEAR> sets "max.". This parameter determines primarily the addition rate outside the control range, see page 21. The maximum rate depends on the Exchange Unit: Exchange Unit max. rate 5 mL 15 mL/min 10 mL 30 mL/min 20 mL 60 mL/min 50 mL 150 mL/min – Direction is set automatically (+, –, auto) auto: The direction is set automatically by the Titrino. +: Direction of higher voltage (more "positive"), larger currents. –: Direction of lower voltage, smaller currents. 0 s Pause 1 (0...999999 s) Waiting time before start volume, e.g. for equilibration of the electrode after start. The waiting time can be aborted with <QUIT>. 795 KFT Titrino 2.6 Parameters, key <PARAM> start V: Type of start volume (OFF, abs., rel.) "OFF": start volume switched off "abs.": absolute start volume in mL "rel.": relative start volume to sample size. OFF cond. start V 0.0 ml cond. factor 0 cond. dos.rate max. ml/min **titr. pause 2 0 s Extraction time (0...999999 s) During this time the titration is running. It will not be stopped (also if EP is already reached), before the extraction time is terminated. The extraction time can be aborted with <QUIT>. I(pol) 50 µA U(pol) 400 mV temperature OFF 25.0 °C cond. time interval cond. 795 KFT Titrino Dosing rate for start volume (0.01...150 mL/min, max.) <CLEAR> sets "max.". The maximum rate depends on the Exchange Unit: Exchange Unit max. rate 5 mL 15 mL/min 10 mL 30 mL/min 20 mL 60 mL/min 50 mL 150 mL/min Pause 2 (0...999999 s) Waiting time after start volume, e.g. reaction time after dosing of a start volume. The waiting time can be aborted with <QUIT>. **titr. electrode test: If "rel." is set: Factor for relative start volume (0...±999999). Calculated as: start V in mL = factor ∗ sample size 0 s **titr. extr.time If "abs." is set: Absolute start volume (0...999.99 mL) 2 s Polarization current (–127...127 µA) or the polarization potential (–1270...1270 mV, in steps of 10 mV) is inquired. Electrode test (OFF, ON) Test for polarized electrodes. Performed on changeover from the inactive standby state to a measurement. "OFF" means that the test is not performed. Titration temperature (–170.0...500.0 °C). The temperature can be entered manually. Time interval (1...999999 s) Time interval for acquisition of a measured value into the measuring point list. 17 2.6 Parameters, key <PARAM> Stop conditions for titration If this is not "normal", i.e. after reaching the EP >stop conditions stop V: abs. **titr. stop V 99.99 ml **titr. factor 999999 **titr. filling rate max. ml/min **titr. conditioning: ON display drift: ON cond. OFF cond. drift value If "abs." is set: Absolute stop volume (0...9999.99 mL) If "rel." is set: Factor for relative stop volume (0...±999999) Calculated as: Stop V in mL = factor ∗ sample size Filling rate after titration (0.01...150 mL/min, max.) <CLEAR> sets "max.". The maximum rate depends on the Exchange Unit: Exchange Unit max. rate 5 mL 15 mL/min 10 mL 30 mL/min 20 mL 60 mL/min 50 mL 150 mL/min Preselections for the sequence >preselections drift corr: Type of stop volume (abs., rel., OFF) "abs.": absolute stop volume in mL "rel.": relative stop volume to sample size "OFF": stop volume switched off. Stop volume is not monitored. The stop volume applies for one single titration. The conditioning volume is not monitored. 0.0 µl/min Automatic conditioning of titration vessel (ON, OFF) If conditioning is "ON", the solution is constantly kept at the endpoint. When conditioning is performed, the volume drift can be displayed during the conditioning: Display of drift during conditioning (ON, OFF). Volume drift. Type of drift correction (auto, man., OFF) Type of drift correction: (EP – drift ∗ time) auto: drift value at start is valid man.: see below OFF : no correction Value for manual drift correction (0.0...99.9 µL/min) cond. req.ident: cond. 18 OFF Request of identifications after start of titration (id1, id1&2, all, OFF) After start, sample identifications can be requested automatically: Only id1, id1 & id2, all three id's or no inquiries. 795 KFT Titrino 2.6 Parameters, key <PARAM> req.smpl size: OFF Request of sample size after start of titration (value, unit, all, OFF) "all" the value and the unit will be requested. OFF Limiting value check for sample size (ON, OFF) With "ON" the error message "sample size out." appears if the entry is outside the set limits. The limiting values are shown in the display window. The absolute value of the limit is checked during sample size input and during the calculation of the results. cond. limit smpl size: cond. low lim. 0.0 If "ON" has been set: Lower limit for sample size (0.0...999 999) 999999 Upper limit for sample size (0.0...999 999) cond. up lim. cond. oven: no cond. activate pulse: cond. 795 KFT Titrino OFF Connected oven (COM1, COM2, no) COM of the Titrino to which the oven is connected. If an oven is connected via RS232 an inquiry will be made for the oven results and these will be inserted into the result report of the Titrino. The report output on the oven must be switched OFF (see also page 115). Set "no" if no oven has been connected or if you have not connected the oven to Titrino the via RS232 interface. Pulse output on I/O line L6 (L6, pin 1) of the remote socket (first, all, cond., OFF) e.g. start of a Dosimat, see page 126. 19 2.6 Parameters, key <PARAM> Titration sequence of KFT <START> (Activate pulse) (Stirrer ON) (Start delay) (Preconditioning) (<START> (Activate pulse) (Start delay) After the start, the activate pulse is outputted and the stirrer switched on. The start delay time is waited off. If conditioning is on, the sample solution is titrated until the EP is reached. The display shows then drift OK or KFT 2.3 µl/min conditioning The vessel is now conditioned. The titration can be started with <START>. (Request ident.) (Request smpl size) (Start conditions) (Extraction time) Titration with test of stop criterion Pause 1 is waited off, the start volume is dispensed and pause 2 waited off. The titration is executed. If the extraction time is not yet over when the endpoint has been reached, the titration will only be terminated after the extraction time is over. (Stirrer OFF) The stirrer is switched off when there is no conditioning. Calculations Calculations are carried out. Data output Data are outputted. (Reconditioning) 20 The sample identifications and the sample size are requested. Conditioning is carried out. 795 KFT Titrino 2.6 Parameters, key <PARAM> Control parameters for KFT The control parameters can be set according to your samples. The default parameters are already set to get satisfactory results. Optimize the control parameters for specific samples only. During the titration, reagent dosing is carried out in 3 phases: U/mV 1. Initial dosing: Here the dosing rate increases constantly up to "max.rate". KFT Ipol EP V/mL t/s V/mL Initial dosing Continuous dosing 2. Continuous dosing: Dosing is performed at the maximum rate "max.rate" until the control range (dynamics) is reached. 3. Control range (dynamics): In this range, dosing is performed in single steps. The last dosing steps are controlled by the parameter "min.volume incr.". Control range I/uA EP KFT Upol V/mL Remarks: • Titer determination should have the same modes and the same parameters as the sample titrations. • In most cases the preset default parameters provide precise and reproducible results. • Ipol gives relatively steep curves. They are flatter with Upol. 795 KFT Titrino 21 2.6 Parameters, key <PARAM> Mechanisms of the KFT parameters in Ipol mode U/mV + Excess H2O Titration (direct titration) EP at U Excess Iodine- Titration (Back titration) I(pol) darker solution + I/µA • The position and curve characteristics of the line between the ranges of excess water or excess iodine depends on the type of sample and the ingredients of the working media. • The endpoint has to be set close to the range margin, but always within the iodine excess range. If the endpoint is set too close to the limit, an overdose of KF reagent may be dispensed. The steeper the curve at the preset polarization current I(pol), the more delicate it is to titrate to a steady and reproducible endpoint. For the titration of troublesome samples, the particular conditions must be optimized by trial and error. Always mind the color of the working medium at the end point as your guideline. Remark: In most cases the preset default parameters provide precise and reproducible results. • If you select negative values for a parameter, you should choose negative values for all other parameters too in order to have compatible parameter sets. • In KFT Upol mode, all parameters work in a similar manner as in KFT Ipol mode. 22 795 KFT Titrino 2.6 Parameters, key <PARAM> The determination of the free water is easily done, as far as the specifications of the reagent manufacturer regarding the "water capacity" of the reagents are considered. Problems may occur with specific sample matrices. The relevant literature contains many precise analysis instructions. Here, we give you some useful hints for the sample addition. Sample addition For sample addition various accessories are available, for example injection syringes, weighing spoons etc. It is a good idea to apply the back-weighing technique, except when you are disposing small amounts of liquids with a micro-syringe. Fill the syringe or the weighing spoon with your sample just before the titration (e.g. during conditioning) and tare it on a balance with an appropriate precision, which ideally is connected to the Titrino. Sample size request should always be switched on (see page 19). Add the sample during the request for the sample size, and weigh the syringe or weighing spoon again to evaluate the weight difference. Use the transfer of balance data to enter the correct sample size if possible. The weight has to be transmitted in gram. If you transfer the sample size from the balance, the sample size request is confirmed automatically, and the titration is started at once. Otherwise use the keypad to enter the weight. If the sample size request is switched off, and preconditioning is set, you are explicitly prompted to add your sample. For six seconds, the message "add sample" is displayed after which the titration is started by the Titrino itself. This waiting time can be extended by pressing <MEAS/HOLD>. Solid samples Use the glass weighing spoon 6.2412.000 and dispose the sample through the opening for the septum stopper. Liquid samples Use a disposable syringe (2...20 mL) or a micro-syringe with a long needle attached. Puncture the septum and dispose the sample carefully. When using disposable syringes, add the liquid sample carefully without dipping into the solvent. Draw back the last drop of sample into the syringe before you redraw the needle. For disposing an exact, small volume of liquid sample, use a micro-syringe. Proceed as described above, but dip the needle into the preconditioned solvent and dispose the sample carefully. Here drawing back of solvent or sample adhering to the needle is not recommended. Always keep in mind to exchange the septum as soon as it shows any large punctures impairing the tightness of the titration cell. Pasty, viscous samples For samples which cannot be disposed with a needle because of their high viscosity, you can handle your samples with disposable syringes with a large volume without using a needle. Dispose your sample through the opening of the septum stopper. Back-weigh the syringe after addition of the sample. Be sure to wipe off any adhering excess sample substance of the syringe before taring it. In any case, pay attention to prevent the penetration of atmospheric moisture into the titration vessel when you are disposing the sample. If you still have to open the titration cell for any reason, determine a blank value and take it into account for the calculation of the titration result (see page 132). 795 KFT Titrino 23 2.6 Parameters, key <PARAM> In the following table we attempt to show you solutions related more to the instrument's side: What to do if ... Problem Dosing at end too long and increments too small. "Is never finished!" Possible causes and remedial action • Increase "min.volume incr.". • Change stop criterion. Try to increase stop drift or use a short stopping time as stop criterion, e.g. • For problematic samples change solvents with ketones or aldehydes in 2-methoxyethanol or with amines mixture in methanol/glacial acetic, e.g., see literature. The increments at the end of the • Lower "max.rate". The following experiment gives you titration are too large. a reference point for the optimum max.rate: Drift "Overshoots". display during conditioning and add sample without starting the titration. Select a value below the maximum drift as "max.rate". • Optimize setup of electrode and buret tip and improve stirring. 24 Solution becomes too brown at the end of the titration. • The methanol fraction in the solvent is too low. Change the solvent. • Electrode could be coated; wipe off with acetone. Solution becomes darker with every titration. • Renew solvent. • Electrode could be coated; wipe off with acetone. The drift increases with every titration. • Does your sample evolve water extremely sluggishly? Work with the KF oven. • Are acids esterified in your sample? Change solution more frequently. Increase buffer capacity of the solvent. • Does your sample contain ketones or aldehydes? Use special reagents suitable for ketones and aldehydes. The endpoint is reached "too rapidly". • Reduce "max.rate". The titration times become longer and longer. • With 2-component reagents the buffer capacity of the solvent can be exhausted. Change solution. • If the drift increases at the same time, see above. 795 KFT Titrino 2.7 Result calculations 2.7 Result calculations Formula entry, key <DEF> DEF 2 ( def >formula >silo calculations >common variables >report >mean >formula Key <DEF> contains various inquiries for result calculations and data output. The data of this key are method specific and they are stored in the method memory together with the method. formula: Formulas for result calculations. The display texts of the Titrino are shown on the left side. The values are the default values. Input of formulas RS? Enter formula number (1...9) You can calculate up to 9 results per method. Enter a number 1...9. RS1= Input of formula Example: RS1=EP1∗C01/C00 Enter formula by means of 3rd functions of keyboard. Here you will find operands, mathematical operations and parentheses. Operands require a number as an identification. You can use the following operands: EPX: EP's. X = 1...9 RSX: Results which have already been calculated with previous formulas. X = 1...9 CXX: Calculation constants. XX = 00...45 RS1=EP1∗C01/C00 Rules: • Calculation operations are performed in the algebraic hierarchy: ∗ and / before + and –. • Store formula with <ENTER>. • Calculation quantities and operands can be deleted with <CLEAR> one by one. • To delete a complete formula press <CLEAR> repeatedly until only RSX remains in the display. Confirm with <ENTER>. If a formula is stored with <ENTER>, result text, number of decimals, result unit and the settings of the result limit control will be requested: 795 KFT Titrino 25 2.7 Result calculations RS1 text RS1 Text for result output (up to 8 characters) Text input see page 8. RS1 decimal places 2 Number of decimal places for result (0...5) RS1 unit: % Selection of result unit (%, ppm, g/L, mg/mL, mol/L, mmol/L, g, mg, mL, mg/pc, s, mL/min, no unit or up to 6 characters). RS1 limit control: OFF RS1 low lim. 0.0 RS1 up lim. 0.0 RS1 L13 output: OFF Limit control for the result (ON, OFF) The limits are checked each time a result is calculated. If "ON" has been set: Lower limit (0.0...999 999) Upper limit (0.0...999 999) Sets line L13 of the remote socket (OFF, active, pulse) if the result lies outside the limits. Enter next formula, e.g. for RS2. Meaning of the calculation variables CXX: C00 Sample size, see page 37. C01...C19 Method specific operands, see page 27. They are stored with the method in the method memory. C21...C23 Sample specific operands, see page 37ff. C26, 27 Mean values from silo calculations, see page 41ff. C30...C39 Common variables. C40 Initial measured value of the sample. C41 End volume. C42 Determination time. C43 Volume drift for KFT with conditioning. C44 Temperature. C45 Dispensed start volume. 26 795 KFT Titrino 2.7 Result calculations Input of method specific operands C01...C19, key <C-FMLA> C-FMLA 1 With <C-FMLA> the operands C01...C19 can be put in. For the calculation, the operands are used, which were introduced in the formula. The inputs method specific and are store in method memory. C The calculation report can be printed with the key sequence <PRINT><←/→> (press keys repeatedly until "calc" appears in the display) <ENTER>. Example for a calculation report: Calculation report 'fm 795 KFT Titrino user date KFT 01103 795.0010 pkl 2001-11-15 Ipol time 15:01 KF-Blank >calculations Water=(EP1-C38)*C39*C01/C00/C02;2;% Titer=C39;4;mg/ml 3 mode und method name formulas: result name=formula;number of decimal places;result unit Blank=C38;4;ml C00= 1.0 C01= 0.1 C02= 1 C38= 0.0 C39= 0.0 sample size method specific operands values of the common variables that are used ------------ 795 KFT Titrino 27 2.8 Statistics calculation 2.8 Statistics calculation Mean values, absolute and relative standard deviations are calculated. DEF 2 The <DEF> key is used to allocate results for statistics calculation. The entries are specific to the method and are stored in the method memory. ( def >formula >silo calculations >common variables >report >mean mean: Assigns values for statistics calculations. The display texts of the Titrino are shown on the left side. The values are the default values. Allocations for statistics calculations >mean Number n of single values for statistics calculation. (1...9) You can perform statistics calculation using up to 9 results (RSX), endpoints (EPX) or variables (CXX). For MN1, the default value RS1 is entered. Delete allocation with <CLEAR> + <ENTER> MN1=RS1 MN2= : MN9= Each mode has an inquiry group ">statistics" in key <PARAM> PARAM Statistics calculation >statistics status: mean res.tab: delete 28 Status of statistics calculation (OFF, ON) If the statistics calculation is switched off, the following inquiries regarding the statistics do not appear. OFF n= 2 original n= 1 Mean value calculation from n single results (2...20) Result table (original, delete n, delete all) "original": The original table is used. Deleted individual results are again incorporated in the evaluation. "delete n": Deletion of single results with the index n. "delete all": The entire table is deleted. Delete data from sample number n (1...20) The deleted result is removed from the statistics calculation. 795 KFT Titrino 2.8 Statistics calculation How do you obtain statistics calculations? 1) Enter the allocations for the statistics calculation, see page 28. 2) Switch on the statistics calculations: Either with <STATISTICS> or set the status under <PARAM>, "> statistics" to "ON". The "STATISTICS" LED is on. Storing a method in the method memory, the status of the statistics calculation is retained. 3) Change the number of the individual values n under "mean n", if necessary. 4) Perform at least 2 titrations. The statistics calculation are constantly updated and printed. The values are printed in the short and full result report. 5) The statistics report can be printed with <PRINT><STATISTICS><ENTER>. Rules: • Recalculated results are incorporated in the statistics calculation. • If a result of a particular titration can not be calculated, no results for this determination are incorporated in the statistics calculation. However, the sample counter is still operative, i.e. the statistics calculation start afresh when the number of required individual determinations has been performed. • If the statistics are switched off ("statistics" LED no longer on), results are no longer entered in the statistics table. But the table remains unchanged. When the statistics are switched on again, you can immediately continue working. • If you delete results, all results of the determination with index n are removed from the statistics evaluation. • On method change, the old statistics table is cleared and the statistics instructions of the new method are followed. • Old results in the statistics table can be deleted with "delete all" (<PARAM>, ">statistics", "res.tab:"). 795 KFT Titrino 29 2.9 Common variables 2.9 Common variables Common variables are used for: • Determination of a titer with a method. This titer is stored permanently as C3X. The operand C3X can be used in various other methods like any other operand. • Determination of a blank values with a method . Using this blank value in various other methods. • Determination of a result with method. Reconciliation of this result in various other methods. You may enter and view the values of the common variables with <CONFIG>. DEF ( 2 def >formula >silo calculations >common variables >report >mean >common variables C30= C31 : C39= 30 With <DEF>, results (RSX), endpoints (EPX), variables (CXX) or mean values (MNX) can be allocated as common variables. The entries are specific to the method and are stored in the method memory. common variables: Assigns values to common variables. The display texts of the Titrino are shown on the left side. The values are the default values. Allocation for common variables Common variable C30...C39 (RSX, EPX, CXX, MNX) Results (RSX), endpoints (EPX), variables (CXX), and means (MNX) can be assigned. The values of the common variables remain in force for all methods until they are overwritten or deleted. They can be viewed under the <CONFIG> key. Delete allocation with <CLEAR>+<ENTER>. 795 KFT Titrino 2.10 Data output 2.10 Data output 2.10.1 Reports for the output at the end of a determination DEF ( 2 With <DEF>, the report sequence at the end of the determination is defined. The entries are specific to the method and are stored in the method memory. def >formula >silo calculations >common variables >report >mean report: Definition of report blocks to be printed automatically at the end of the determination. >report Report sequence The display texts of the Titrino are shown on the left side. The values are the default values. report COM1: Report sequence for COM1: full, short, mplist, curve, scalc full, scalc srt, param, calc, ff report COM1:full;curve Select a block using the keys <←> and <→>. If you require more than one report block, set a ";" as a delimiter between the blocks. Identical for COM2. Meaning of the report blocks: param Parameter report. full Full result report with raw results, calculations and statistics. short Short result report with calculations and statistics. mplist Measuring point list. curve Curve volume vs. time scalc full Full report of silo calculations. scalc srt Short report of silo calculations. calc Report with formulas and operands. ff Form feed on printer. 795 KFT Titrino 31 2.10 Data output Original reports which are put out automatically at the end of the titration can be printed with recalculated values at any time. Key sequence: <PRINT><REPORTS><ENTER>. Original reports have double dashes ==== at the end, whereas recalculations are marked by single dashes ----. Report outputs can be stopped with <QUIT>. Example of reports: Full result report 'fr 795 KFT Titrino 01103 user 795.0010 pkl date 2001-11-15 KFT Ipol time 15:01 KF smpl size 0.879 g EP1 2.5725 ml Water 1.44 % Titer 4.9372 mg/ml mean( 3) Water +/–s 1.46 device label s/% 0.027 % Titr 1 1.86 sign: ============ 01103 user 5.0 Device label (if there is a designation, see page 11) and manual signature. Curve 'cu 795 KFT Titrino date User (only if entered) 3 795.0010 pkl 2001-11-15 s/div time 15:01 3 KFT Ipol KF Scaling of time axis dV=0.5 ml/div ============ 32 795 KFT Titrino 2.10 Data output Additional possibilities for report outputs In addition to the reports which are printed at the end of the titration, various other reports can be put out. There are 2 possibilities to select the reports: 1) <PRINT><←/→><ENTER> 2) <PRINT><keyX><ENTER> are entered. Cursor is pressed repeatedly until the desired report appears in the display. key X is the key under which the appropriate data List of the "keys X": Report Configuration report Parameter report Current sample data Statistics report with the individual results All sample data from the silo memory Operands C01...C19 Contents of the <DEF> key Contents of the method memory with details of the memory requirements of the individual methods and the remaining bytes Complete report sequence of the last determination, as defined under the <DEF> key in the method <Key X> CONFIG PARAM SMPL DATA STATISTICS SILO C-FMLA DEF USER METH REPORTS Result display without printer If you work without printer, we recommend to work with the standard character set for result display (settings in key <CONFIG>, ">auxiliaries", see page 11). You will get the complete information on your determinations: Calculated results, endpoints, messages etc. 2.10.2 Display of the Curve After the titration, the curve can be viewed. Switch between "curve" and "result display" with key <CURVE>. You can trace the curve with keys <↑> and <↓>. In the text field on the left side of the curve the index of the current measured value is displayed in the first line. In the subsequent lines, the corresponding measured values are shown. 795 KFT Titrino 33 2.11 User name, key <USER> 2.11 User name, key <USER> USER The key <USER> manages the user names. User names can be entered directly or selected with the keys <←> and <→>. + ← user name: >delete boss name: Selection or input of user name. delete: Delete user name. The display texts of the Titrino are shown below at the left. name: >delete name: 34 User name (up to 10 ASCII characters) User names can be entered directly or selected with the keys <←> and <→>. The user name is printed out in the report. The user name remains in the instrument until it is deleted (or until the RAM is initialized). If no operator name is to be printed out the user "blank" can be selected. Delete user name Enter the name directly or select it with the keys <←> and <→>. <ENTER> will delete the name from the list of user names. 795 KFT Titrino 2.12 Method memory key <USER METH> 2.12 Method memory key <USER METH> USER METH 3 user methods >recall method >store method >delete method ) Management of the internal method memory with key <USER METH>. Select method name with keys <←> and <→>. recall method: Loads a method from the internal method memory into the working memory. store method: Stores the method which is in the working memory in the internal method memory. delete method: Deletes a method from the internal method memory. The display texts of the Titrino are shown on the left side. The values are the default values. >recall method method name: >store method method name: 795 KFT Titrino Recall method Recall method from the internal method memory to the working memory (input of method name, which is included in the memory). If a method identification is entered which is not found in the method memory, the selected value blinks. Store method Store method from the working memory to the internal method memory (up to 8 ASCII characters). If a method with an identical name is already stored, you are requested if you wish to overwrite the old method. With <ENTER> it is overwritten, with <QUIT> you return to the entry. 35 2.12 Method memory key <USER METH> >delete method method name: Delete method Delete method from the internal method memory (input of method name, which is included in the memory). For safety, you are again asked if you really wish to delete the method. With <ENTER> it is deleted, with <QUIT> you return to the working memory. If a method name is entered which is not found in the method memory, the selected value blinks. The contents of the method memory can be printed with the key sequence <PRINT><USER METH><ENTER> Document your methods (e.g. parameter report, def. report and C-fmla report)! With a PC and the 6.6008.XXX Vesuv program, you should carry out a complete method backup periodically. 36 795 KFT Titrino 2.13 Current sample data, key <SMPL DATA> 2.13 Current sample data, key <SMPL DATA> The key <SMPL DATA> can be used to enter the current sample data. The content of this key changes when the silo memory is switched on, see page 39. Instead of entering the current sample data with <SMPL DATA>, you can request these data automatically after start of determinations. Configuration: <PARAM>, ">preselections". Current sample data can be entered live. For working with the silo memory see page 38. id#1...3 or C21...C23, sample identifications: The sample identifications can also be used as sample specific calculation variables C21...C23. smpl size: Sample size. The sample size can be monitored, see e.g. page 19. The limits are then displayed in this window. smpl unit: Unit of the sample size. SMPL DATA smpl data id#1 or C21 id#2 or C22 id#3 or C23 smpl size smpl unit: 1.0 g g The display texts of the Titrino are shown on the left side. The values are the default values. Sample data smpl data Sample identification 1...3 or sample specific operand C21...C23 (up to 8 characters). Sample identifications or sample specific operands can be entered using the keypad, via a balance with a special input device or via barcode reader. id#1 or C21 id#2 or C22 id#3 or C23 smpl size smpl unit: 795 KFT Titrino 1.0 g g Sample size (6-digit number: ±X.XXXXX) Entry using keypad, via a balance or via barcode reader. Unit of sample size (g, mg, mL, µL, pc, no unit or up to 5 characters) Select unit with <←/→>. 37 2.14 Silo memory for sample data 2.14 Silo memory for sample data In the silo memory or pushup storage, sample data (method, identifications and sample size) can be stored. This is useful, e.g. when you work with Sample Changers and other automatic sample addition systems or if you wish an overview of your determination results, see page 41. SILO 9 Press the key <SILO> for working with the silo memory. The status LED "silo" is on when the silo memory is switched on. The silo memory works by the FIFO principle (First In, First Out). - If the silo memory is switched on, sample data are routed to the last free line of the silo memory. If no new value is put in, the value from the last line is automatically copied. In this manner, data can be simply taken over when they remain unchanged. When the instrument is started, the sample data are fetched from the next silo line. Organization of the silo memory 255 1 255 2 1 2 6 35 Silo memory contains 35 lines. Next free line is 36 35 6 of the 35 lines have been processed. Free lines from 36 to 255 and from 1 to 6. 1 silo line needs between 18 and 120 bytes memory capacity. Filling the silo memory with a connected balance If the silo memory is filled from the balance, you must ensure that there is sufficient space in the silo memory for the required number of silo lines! The number of free bytes is given in the user memory report. When the sample data are entered from a balance, the transfer of the sample size is taken as the end of the silo line. You should not send data from the balance and edit the silo memory at the same time. For mixed operation, manual input of identifications and sample sizes from a balance, the values from the balance are sent into the line in which editing just takes place. Confirmed the data with <ENTER> at the Titrino. 38 795 KFT Titrino 2.14 Silo memory for sample data Key <SMPL DATA> with the silo memory switched on Sample data can be entered into the silo memory with key <SMPL DATA>. SMPL DATA edit silo lines: Entering sample data into the silo memory. delete silo lines: Deletes single silo lines. delete all silo lines: Deletes the whole silo memory. smpl data >edit silo lines >delete silo lines >delete all silo lines cycle lines: OFF save lines: OFF The display texts of the Titrino are shown on the left side. The values are the default values. Input for silo memory >edit silo lines silo line 1 Silo line (1...255) The next free line is displayed automatically. Lines already occupied can be corrected. method: Method with which the sample is processed (method name from the method memory) If no method name has been entered, the sample is processed with the method in the working memory. Selection of the method with <←/→>. id#1 or C21 Sample identification 1...3 or sample specific calculation variables C21...C23 (up to 8 characters) id#2 or C22 id#3 or C23 smpl size smpl unit: 1.0 g g 795 KFT Titrino Unit of sample size (g, mg, mL, µL, pc, no unit or up to 5 characters) Select unit with <←/→>. Delete individual silo lines >delete silo lines delete line n Sample size (6-digit number: ±X.XXXXX) The method specific limits are tested on result calculation. OFF Line number of the line to be deleted (1...255, OFF) <CLEAR> sets "OFF". Deleted lines remain in the silo memory. Access is blocked during the processing. To show that a line has been deleted, they are marked with "∗". The symbol ∗ indicates that the line has been deleted. Deleted lines can be reactivated if the appropriate line is re-edited. 39 2.14 Silo memory for sample data Delete all silo lines >delete all silo lines delete all: Confirmation (yes, no) When all silo lines are deleted, the silo is completely empty: The line numbering starts again with 1. no cycle lines: OFF With "ON", worked off silo lines will be copied to the highest line of the silo memory (ON, OFF) Data cycling "on" is useful if you constantly have to process the same sample data. In such a case, the processed silo line is not deleted, but copied to the next free line, see below. If you work in this mode, you should not enter any new silo lines during the determinations. save lines: OFF Store results in the silo memory (ON, OFF) Determination results will be stored as C24 or C25 in the silo memory according to the allocations in the methods, see page 42. "save lines" can only be set to "OFF" if the silo is completely empty. Silo memory with data cycling "on" 255 1 255 2 1 2 6 35 35 41 Silo memory contains 35 lines. Next free line is 36. 40 6 of 35 lines have been processed. The processed lines have been copied to the end of the silo memory: your silo is filled up to line 41. 795 KFT Titrino 2.15 Storing determination results and silo calculations 2.15 Storing determination results and silo calculations 2.15.1 Storing determination results If the sample-specific data of the silo memory should be kept after the determination and supplemented by results, the following entries are necessary: 1. In the method under <DEF> Assignment of the determination results to C24 and/or C25: 2. In the silo memory, <SMPL DATA> (when the silo memory is switched in): "save lines: on" Assignment of determination results DEF 2 ( The determination results are assigned in key <DEF>. The display texts of the Titrino are shown on the left side. def >formula >silo calculations >common variables >report >mean >silo calculations C24= C25= Silo calculations Assignment to C24 (RSX, EPX, CXX) Calculated results (RSX), endpoints (EPX) or variables CXX can be stored as C24. Same procedure for C25. Important: Ensure that there is still sufficient space for storing the results C24 and C25. (In the report <PRINT><USER METH><ENTER> the number of free bytes is shown.) Result name, value and unit are stored. The memory requirements can be estimated as follows: Result with text (8 characters) and unit (5 characters): 32 bytes Measured value C40, value without unit: 22 bytes 795 KFT Titrino 41 2.15 Storing determination results and silo calculations After several samples have been processed, the silo memory report can have the following appearance (printout with <PRINT><SILO><ENTER>): 'si 795 KFT Titrino date 01103 2001-11-15 time 795.0010 15:03 14 >silo cycle lines: OFF save lines: sl method ON id 1/C21 id 2/C22 id 3/C23 C00 C24 C25 + 1 11-2 A/12 99-08-12 0.903g 2.6427ml 1.48% + 2 11-2 A/13 99-08-12 0.891g 2.6076ml 1.46% / 3 11-2 A/14 99-08-12 0.879g 2.5725ml 1.44% 4 11-2 A/15 99-08-12 0.913g NV NV 5 11-2 A/16 99-08-12 0.888g NV NV processed silo lines with saved results The silo lines can be marked as follows (at very left of report): + Silo line has been processed. It cannot be edited anymore. ∗ A silo line not yet processed has been deleted. – A processed silo line has been deleted and hence removed from the silo calculations. / The last processed silo line. Recalculation will be considered e.g., if the sample data of this line are changed. No marking: The silo line is awaiting processing. For silo lines ≥100, the first digit will be overwritten by the marking. 2.15.2 Silo calculations Mean value and standard deviation of the results available in the silo memory can subsequently be calculated over the entire series. The following details can be entered in the method under <DEF>: Silo calculations >silo calculations Assignment to C24 and C25 Calculated results (RSX), endpoints (EPX) and variables (CXX) can be stored as C24. Identical for C25. C24= C25= match id: 42 OFF Which sample identifications must match in order to combine of the results (id1, id1&2, all, OFF) "OFF" means no matching ids, all samples which have been processed with the same method are combined, see examples below. 795 KFT Titrino 2.15 Storing determination results and silo calculations Starting from the following silo report: 'si 795 KFT Titrino 01103 date time 2001-11-15 795.0010 15:03 14 >silo cycle lines: OFF save lines: ON sl method id 1/C21 id 2/C22 id 3/C23 + 1 11-2 A/12 99-08-12 0.903g C00 2.6427ml C24 C25 + 2 0-15 A/13 99-08-12 0.010g 4.9372mg/ml + 3 0-15 A/13 99-08-12 0.010g 4.9786mg/ml + 4 11-2 A/12 99-08-12 0.852g 2.4935ml 1.39% / 5 11-2 A/15 99-08-12 0.913g 2.6720ml 1.50% 1.48% NV NV ∗ Assignment for C24 only ∗ ∗ with "match id: off" the following silo calculation report (scalc full) is obtained: : method 11-2 id 1/C21 id 2/C22 id 3/C23 * * mean * Consum. Content 0-15 * * * Titer 2.6027ml 1.46% 4.9579 +/–s n 0.0957 3 0.06 3 0.0293 2 All samples which have been processed with the same method are combined With "match id: id1" the following silo calculation report (scalc full) is obtained: : method 11-2 id 1/C21 id 2/C22 id 3/C23 A/12 * mean * Consum. Content 0-15 A/13 * * Titer 11-2 A/15 * * Consum. Content +/–s n 0.1055 2 0.06 2 0.0293 2 2.6720ml 0.000 1 1.50% 0.000 1 2.5681ml 1.44% 4.9579 Sample processed with the same method and having the same id1 are combined The short silo calculation report contains only calculations for the current sample. : method 11-2 id 1/C21 id 2/C22 id 3/C23 A/15 * mean * Consum. Content +/–s n 2.6720ml 0.000 1 1.50% 0.000 1 The mean values of the silo calculations are available for further result calculations as C26 and C27 and can be used in the Titrino in formulas. Mean value of C24 ⇒ C26 Mean value of C25 ⇒ C27 Important: • If work is performed with silo calculations, the method name must be entered in the silo memory. • Results will be overwritten in the silo recalculation, as long as the silo line is marked with "/". If you do not wish such an input, e.g. because you work off an urgent sample between a series, disconnect the silo. 795 KFT Titrino 43 2.16 Manual dosing • Calculations and assignments are carried out in the following order: 1. Calculation of the results RSX 2. Calculation of means MNX 3. Assignment of silo results C24 and C25 4. Silo calculations 5. Assignment of means C26 and C27 from silo calculations 6. Assignment of common variables C3X 2.16 Manual dosing DOS 44 With <DOS>, the internal buret will dose as long as <DOS> is pressed. The dosing rate can be set with the analog potentiometer at the Titrino. 795 KFT Titrino 3.1 General rules 3 Operation via RS232 Interface 3.1 General rules The Titrino has an extensive remote control facility that allows full control of the Titrino via the RS 232 interface, i.e. the Titrino can receive data from an external controller or send data to an external controller. CR and LF are used as terminators for the data transfer. The Titrino sends 2xCR and LF as termination of a data block, to differentiate between a data line which has CR and LF as terminators. The controller terminates its commands with CR and LF. If more than one command per line is sent by the controller, ";" is used as a separator between the individual commands. The data are grouped logically and easy to understand. Thus e.g., for the selection of the dialog language, the following must be sent &Config.Aux.Language "english" whereby it is sufficient to only transmit the boldface characters, thus: &C.A.L "english" The quantities of the commands above are: Config configuration data Aux auxiliaries, various data Language setting the dialog language The data are hierarchically structured (tree form). The quantities that occur in this tree are called objects in the following. The dialog language is an object which can be called up with the &Config.Aux.Language command. If one is in the desired location in the tree, the value of the object can be queried. &Config.Aux.Language $Q Q means Query The query command $Q initiates the issuing of the value on the instrument and the value emission is triggered. Entries which start with $, trigger something. They are thus called triggers. Values of objects can not only be queried, they can also be modified. Values are always entered in quotes, for example: &Config.Aux.Language "english" 795 KFT Titrino 45 3.1 General rules 3.1.1 Call up of objects An excerpt from the object tree is represented below: 3rd node Language 2nd node 1st node Prog Aux RSSet Config Mode 0st node & Root Rules Example The root of the tree is designated by &. The branches (levels) of a tree are marked with a dot (.) when calling up an object. When calling up an object, it is sufficient to give only as many letters as necessary to uniquely assign the object. If the call is not unequivocal, the first object in the series will be recognized. Calling up the dialog language Upper- or lowercase letters may be used. &C.A.L or &c.a.l To an object a value can be assigned. Values are signified at the beginning and end by quotes ("). They may contain up to 24 ASCII characters. Numerical values can contain up to 6 digits, a negative sign, and a decimal point. Numbers with more than 6 characters are not accepted; more than 4 decimal places are rounded off. For numbers <1, it is necessary to enter leading zeros. Entering the dialog language: &C.A.L"english" The current object remains until a new object is called. entry of another dialog language: "deutsch" &Config.Aux.Language or &C.A.L correct entry of numbers: "0.1" incorrect entry of numbers "1,5" or "+3" or ".1" New objects can be addressed relative to the From the root to node 'Aux': &C.A old object: Forward from node 'Aux' to 'Prog': .P A preceding dot leads forwards to the next level in the tree. More than one preceding dot leads one level backwards in the tree. n node backwards require n+1 preceding dots. If you must jump back to the root, enter a preceding &. 46 Jump from node 'Prog' to node 'Aux' and select a new object 'Language' at this level: ..L Change from node 'Language' via the root to node 'Mode': &M 795 KFT Titrino 3.1 General rules 3.1.2 Triggers Triggers initiate an action on the Titrino, for example, starting a process or sending data. Triggers are marked by the introductory symbol $. The following triggers are possible: $G Go $S $H $C $Q Stop Hold Continue Query $Q.P $Q.H Path Highest Index Name Detail-Info qUit $Q.N"i" $D $U Starts processes, e.g. starting the mode run or setting the RS 232 interface parameters Stops processes Holds processes Continues processes after Hold Queries all information from the current node in the tree forward up to and including the values Queries the path from the root of the tree up to the current node Queries the number of son nodes of the current node Queries the name of the son node with index i, i = 1 – n Queries the detailed status information Aborts the data flow of the instrument, for example, after $Q The triggers $G and $S are linked to particular objects, see the summary table page 52ff. All other triggers can be used at any time and at all locations on the object tree. Examples: Querying the value of the baud rate: &Config.RSSet.Baud $Q Querying all values of the node "RSSet": &Config.RSSet $Q Querying the path of the node "RSSet": &Config.RSSet $Q.P Start mode: &Mode $G Querying the detailed status: $D 795 KFT Titrino 47 3.1 General rules 3.1.3 Status messages In order to have an efficient control by an external control device, it must also be possible to query status conditions; they provide information on the status of the Titrino. The trigger $D initiates output of the status. Status messages consist of the global status, the detailed status and eventual error messages, e.g. $S.Mode.KFT;E26. The global status informs on the activity of the process, while the detailed status conditions show the exact activity within the process. $G $H $C $R $S Go: Hold: Continue: Ready: Stop: The following global status conditions are possible: The Titrino is executing the last command. The Titrino has been held ($H, key <meas/hold> or by an error which effects the hold status). The Titrino has been restarted actively after hold. The Titrino has executed the last command and is ready. A process has been aborted in an "unnatural manner". e.g. stopped or aborted because there was an error. Detailed status conditions Status conditions of the global $G: Instrument at the beginning or at the end of a titration. .Req .Id1: Instrument in the KFT mode, requesting Id1 after start. .Id2: Instrument in the KFT mode, requesting Id2 after start. .Id3: Instrument in the KFT mode, requesting Id3 after start. .Smpl: Instrument in the KFT mode, requesting sample size after start. .Unit: Instrument in the KFT mode, requesting unit of sample size after start. .Start: Instrument in the KFT mode, processing the start conditions. .KFT1: Instrument in the KFT mode, titrating to the first endpoint. .Cond.Ok: Instrument in the KFT, conditioning, endpoint reached (after the first startup from the standby mode). .Cond.Prog: Instrument in the KFT mode, conditioning, endpoint not reached (Conditioning progressing). $G .Assembly.Bur .Fill: Buret in filling process .ModeDis: Buret in DIS mode $G .Mode.KFT .Inac: Status conditions of the global $H: The status message of the action which has been held appears. If the process is held because a monitored limit has been violated, its status message is $H.Mode.KFT.Titr. Status conditions of the global $C: The status conditions of the global $C are identical with the ones of the global status $G. They appear when the process has been restarted actively from the status "Hold" ($C, key <meas/hold> or automatically after elimination of an error). Status conditions of the global $R: Quick manual measurement from the initial status in mode KFT. $R .Mode.KFT .Inac: Instrument in the KFT mode, inactive. .Cond.Ok: Instrument in the KFT mode, conditioning, endpoint reached. .Cond.Prog: Instrument in the KFT mode, conditioning, endpoint not reached. $R .Assembly.Bur.ModeDis: Buret in the DIS mode, inactive. $R .Mode.KFT.QuickMeas: 48 795 KFT Titrino 3.1 General rules Status conditions of the global $S: $S .Mode.KFT.QuickMeas: Quick manual measurement from the initial status in mode KFT. The instrument gives the status from which it has been stopped. The detailed status information is therefore identical the information for the global status $G. Violation of monitored limits with action "end" give the status message $S.Mode.KFT.Inac;EYYY. 3.1.4 Error messages Error messages are added to the status messages and separated from them by the sign ";". E20 E21 E22 E23 E26 E27 E28 E29 E30 E31 E32 E33 E34 795 KFT Titrino Check exchange unit. Exit: Mount Exchange Unit (properly) or &m $S. Check electrode, short circuit. Exit: Rectify fault or &m $S. Check electrode, break. Exit: Rectify fault or &m $S. Division by zero. Exit: The error message disappears on next startup or on recalculation. Manual stop. Exit: The error message disappears on next startup. Stop V reached in KFT. Exit: The error message disappears on next startup. Wrong object call up. Exit: Send correct path for object. Start path at root. Wrong value or no value allowed. Exit: Send correct value or call up new object. Wrong trigger, this trigger is not allowed or carrying-out of action not possible. Exit: Send correct trigger (exception: $D) or call up new object. Command is not possible in active status. Repeat command in inactive status. Exit: Send new command. Command is not possible during titration. Repeat command during the conditioning phase or in inactive status. Exit: Send new command. Value has been corrected automatically. Exit: Send new command. Instrument at the end of the titration and sample data is edited; the instrument at rest or editing during filling. Exit: &m $S. 49 3.1 General rules E36 E37 E38 E39 E42 E43 E45 E121 E123 E128 E129 E130 E132 E133 E137 E155 50 RS receive errors: Parity. Exit: <QUIT> and ensure settings of appropriate parameters at both devices are the same. Framing error. Exit: <QUIT> and ensure settings of appropriate parameters at both devices are the same. Overrun error. At least 1 character could not be read. Exit: <QUIT> The internal working-off buffer of the Titrino is full (>82 characters). Exit: <QUIT> RS send errors: CTS=OFF No proper handshake for more than 1 s. Exit: <QUIT> Is the receiver switched on and ready to receive? The transmission of the Titrino has been interrupted with XOFF for at least 6 s. Exit: Send XON or <QUIT> The receive buffer of the Titrino contains an incomplete command (LF missing). Sending from the Titrino is therefore blocked. Exit: Send LF or <QUIT>. Measuring point list overflow (more than 500 measuring points). Exit: The error message disappears on next startup. Missing EP for calculation. Exit: The error message disappears on next startup or on recalculation. No new mean. Exit: The error message disappears on next startup or on recalculation. No new common variable, old value remains. Exit: The error message disappears on next startup or on recalculation. Wrong sample. For KFT with preset titration direction the first measured value lies behind the endpoint. Exit: The error message disappears on next startup. Silo empty and it has been started with open silo or empty silo has been opened. Exit: Send a silo entry. Silo full. Exit: Send new command. XXX Bytes are missing so that the method or the silo line could not be stored. Exit: Send new command. No new silo result (C24 or C25). Exit: The error message disappears on next start or on recalculation. 795 KFT Titrino 3.1 General rules E196 E197 E198 E199 E203 E212 E213 E214 795 KFT Titrino Result is out of limits. Exit: The error message disappears on next start or on recalculation. Sample size is out of limits. Exit: The error message disappears on next start or on introduction of new sample size. Validation interval is expired. Exit: The error message disappears on next start or clear counter with &Config.Monitoring.Validation.ClearCount $G. Service date is reached. Exit: The error message disappears on next start or change date in &Config.Monitoring.Service.Date. No Oven parameters: Oven not (correctly) connected. Exit: The error message disappears on next start. If you don't wish oven parameters in your report, select &Mode.Parameter.Presel.Oven "no" in your method(s). Transmission error from Remote Box. Unknown characters. Exit: Rectify error and switch Titrino off and on again. Time-out error from PC keyboard (Remote Box) Exit: Rectify error and switch Titrino off and on again. Check Remote Box. Remote Box not (properly) connected but activated in &Config.Periph.RemoteBox. Exit: Rectify error and switch Titrino off and on again. 51 3.2 Remote control commands 3.2 Remote control commands 3.2.1 Overview The internal object tree can be divided into the following branches: & ├ Mode ├ UserMeth ├ Config ├ SmplData ├ Hotkey ├ Info ├ Assembly ├ Setup └ Diagnosis 52 Root Method parameters Administration of the internal user-memory for methods Instrument configuration Sample specific data Keys with direct access Current Data Component data Setting the operating mode Diagnostics program 795 KFT Titrino 3.2 Remote control commands &Mode Object Description & Root ├ Mode : ├ .QuickMeas ├ .Select ├ .KFTQuantity ├ .Name ├ .Parameter* Mode $G, $S, $H, $C Rapid meas. in basic mode $G, $S Mode selection KFT Measured quantity for KFT Ipol, Upol Name of current method read only/read+write Parameter of current mode, see below │ ├ .Def │ ├ .Formulas │ │ ├ .1 │ │ │ ├ .Formula │ │ │ ├ .TextRS │ │ │ ├ .Decimal │ │ │ ├ .Unit │ │ │ ├ .Limits │ │ │ ├ .LoLim │ │ │ ├ .UpLim │ │ │ ├ .Output │ │ │ : │ ├ .SiloCalc │ │ ├ .Assign │ │ │ ├ .C24 │ │ │ ├ .C25 │ │ │ ├ .MatchId │ ├ .ComVar │ │ ├ .C30 │ │ ├ up to C39 │ ├ .Report │ │ ├ .Assign1 │ │ ├ .Assign2 │ ├ .Mean │ │ ├ .1 │ │ │ ├ .Assign │ │ │ : │ ├ .TempVar ├ .CFmla │ ├ .1 │ │ ├ .Value │ ├ up to C19 795 KFT Titrino Definitions for data output Calculation formulas for result 1 Calculation formula Text for result output Number of decimal places Unit for result output Limits for result Lower limit Upper limit Output on L13 up to 9 results Silo calculations Assignment Store as variable C24 Store as variable C25 Matching of Id's Assignment of common variables for C30 Input range 3.2.2.1. 3.2.2.2. 3.2.2.3. ditto 3.2.2.4. special up to 8 ASCII char 0...2...5 up to 6 ASCII char ON, OFF 0...±999 999 0...±999 999 active, pulse, OFF 3.2.2.5. ditto ditto ditto ditto ditto ditto ditto RSX,EPX,CXX RSX,EPX,CXX id1, id1&2, all, OFF 3.2.2.6. RSX,EPX,CXX,MNX 3.2.2.7. Reports at the end of determination Output to COM1 special Output to COM 2 as COM1 Assignment for mean calculation MN1 Input of variable RSX, EPX, CXX without meaning Calculation constants Calculation constant C01 Input of value Reference 0...±999999 3.2.2.8. 3.2.2.9. 3.2.2.10. 53 3.2 Remote control commands *Parameter ├ .CtrlPara │ ├ .EP Endpoint │ ├ .UnitEp │ ├ .Dyn │ ├ .UnitDyn │ ├ .MaxRate │ ├ .MinIncr │ ├ .Stop │ │ ├ .Type │ │ ├ .Drift │ │ ├ .Time │ │ │ │ ├ .StopT ├ .TitrPara │ ├ .Direction │ ├ .XPause │ ├ .StartV │ │ ├ .Type │ │ ├ .V │ │ ├ .Factor │ │ ├ .Rate │ ├ .Pause │ ├ .ExtrT │ ├ .MeasInput │ ├ .Ipol │ ├ .Upol │ ├ .PolElectrTest │ ├ .Temp │ │ ├ │ .TDelta ├ .StopCond │ ├ .VStop │ │ ├ .Type │ │ ├ .V │ │ ├ .Factor │ │ ├ │ .FillRate ├ .Statistics │ ├ .Status │ ├ .MeanN │ ├ .ResTab │ │ ├ .Select │ │ │ │ ├ .DelN ├ .Presel │ ├ .Cond │ ├ .DriftDisp │ ├ .DCor │ │ ├ .Type │ │ ├ .Value │ ├ .IReq │ ├ .SReq │ ├ .LimSmplSize │ │ ├ .Status │ │ ├ .LoLim │ │ ├ .UpLim │ ├ .Oven │ ├ .ActPulse 54 Tree part "Parameters for KFT" Control parameters depends on meas.quant. Unit of endpoint Dynamics Unit of dynamics Maximum dosing rate Minimum increment Titration stop Type of stop criterion Stop drift Switch-off delay time Stop time Titration parameters Titration direction Waiting time before start volume Start volume Type of start volume Volume for absolute start volume Factor for relative start volume Dispensing rate for start volume Waiting time after start volume Extraction time without meaning Polarization current Polarization voltage Test for polarized electrodes Titration temperature Time interv. for meas.acquisition Stop conditions Stop volume Type of stop volume Volume for absolute stop volume Factor for relative stop volume Filling rate Statistics Status of statistics calculation No. of individual determinations Result table Deletion of individual results Preselections Conditioning Display of drift during cond. Drift correction Type of drift acquisition Drift value for manual drift corr. Request of Id's after start Request of smpl size after start Limits for sample size Status of limit control Lower limit Upper limit KF Oven connected Output of a pulse 3.2.2.11. read only ditto depends on meas.quant. 3.2.2.12. read only ditto 0.01...150, max. ditto 0.1...9.9, min. ditto drift, time 1...20...999 0...10...999, inf 0...999999, OFF 3.2.2.13. ditto ditto ditto +, –, auto 0...999999 3.2.2.14. 3.2.2.15. abs., rel., OFF 0...999.99 0...±999999 0.01...150.0, max. 0...999999 0...999999 3.2.2.16. ditto ditto ditto 3.2.2.17. 3.2.2.18. 0...50...±127 0...400...±1270 ON, OFF –170.0...25.0...500.0 1...2...999999 3.2.2.19. ditto ditto 3.2.2.20. 3.2.2.21. abs., rel., OFF 0...99.99...9999.99 0...±999999 0.01...150.0, max. 3.2.2.22. ditto ditto 3.2.2.23. ON, OFF 2...20 3.2.2.24. ditto original,delete n,delete all 1...20 ditto ditto ON, OFF ON, OFF 3.2.2.25. ditto auto, man., OFF 0.0...99.9 id1, id1&2, all, OFF value, unit, all, OFF ditto ditto 3.2.2.26. ditto 3.2.2.27. ditto ditto ditto 3.2.2.28. 3.2.2.29. ON, OFF 0.0...999 999 0.0...999 999 COM1, COM2, no first, all, cond., OFF 795 KFT Titrino 3.2 Remote control commands &UserMeth Object Description Input range Reference & Root : ├ UserMeth : ├ .FreeMemory ├ .Recall │ ├ .Name ├ .Store │ ├ .Name ├ .Delete │ ├ .Name ├ .DelAll ├ .List │ ├ .1 │ │ ├ .Name │ │ ├ .Mode │ │ ├ .Quantity │ │ ├ .DosUnit │ │ ├ .Bytes │ │ ├ .Checksum ├ .2 795 KFT Titrino Method memory Memory available Load method Method name Save method Method name Delete method Method name Delete all methods List of methods Method 1 Method name Mode Measured quantity Dosing element Method size in bytes Checksum of method for each method read only $G 8 ASCII characters $G 8 ASCII characters $G 8 ASCII characters $G 3.2.2.30. 3.2.2.31. ditto ditto ditto ditto ditto ditto read only read only read only read only read only read only 3.2.2.32. ditto ditto ditto ditto ditto 55 3.2 Remote control commands &Config Object Description Input range Reference Instrument configuration Monitoring functions Validation monitoring Status of validation monitoring Time interval for validation Time counter Clears the counter above Monitoring of Metrohm service Status of service monitoring Date of next service Printing of system test report ON, OFF 1...365...9999 0...9999 $G $G ON, OFF YYYY-MM-DD ON, OFF 3.2.2.33. ditto ditto ditto ditto 3.2.2.34. ditto ditto 3.2.2.35. Epson,Seiko,Citizen IBM,HP 3.2.2.36. & Root : ├ Config : ├ .Monitoring │ ├ .Validation │ │ ├ .Status │ │ ├ .Interval │ │ ├ .Counter │ │ ├ .ClearCount │ ├ .Service │ │ ├ .Status │ │ ├ .Date │ ├ .DiagRep │ ├ .PeriphUnit │ ├ .CharSet1 │ │ │ ├ .CharSet2 │ ├ .RepToComport │ ├ .Balance │ │ │ ├ .Stirrer │ ├ .RemoteBox │ │ ├ .Status │ │ ├ .Keyboard │ │ │ │ │ ├ .Barcode │ │ │ │ ├ .Aux │ ├ .Language │ │ │ │ │ ├ .Set │ │ ├ .Date │ │ ├ .Time │ ├ .RunNo │ ├ .AutoStart │ ├ .StartDelay │ ├ .ResDisplay │ ├ .DevName │ ├ .Prog 56 Selection of peripheral units External printer as for CharSet1 Output of manual reports Selection of balance Stirrer control Connected remote box Status Type of keyboard Input of barcode reader Miscellaneous Dialog language Setting of date and time Date Time Run number Automatic start Start delay time Result display Device label Program version 1, 2, 1&2 3.2.2.37. Sartorius,Mettler,Mettler AT AND,Precisa 3.2.2.38. ON, OFF 3.2.2.39. 3.2.2.40. ON, OFF ditto US, deutsch, francais, español, schweiz. ditto input, method, id1, id2, id3, smpl size ditto english, deutsch, français, español, italiano, portugese, svenska 3.2.2.41. $G 3.2.2.42. YYYY-MM-DD hh:mm 0...9999 3.2.2.43. 1...9999, OFF 3.2.2.44. 0...999999 3.2.2.45. standard,bold 3.2.2.46. 8 ASCII char. 3.2.2.47. read only 3.2.2.48. 795 KFT Titrino 3.2 Remote control commands ├ .RSSet1 │ ├ .Baud │ │ │ │ │ ├ .DataBit │ ├ .StopBit │ ├ .Parity │ ├ .Handsh │ │ ├ .RSSet2 │ ├ .ComVar │ ├ .C30 │ ├ up to C39 795 KFT Titrino "Configuration", continuation Settings RS232, 1 Baud rate Number of data bits Number of stop bits Parity Handshake as for RS1 Values of common variables C30 0... ±999999 $G 3.2.2.49. 300,600,1200,2400,4800, 9600,19200,38400,57600, 115200 ditto 7, 8 ditto 1, 2 ditto even, odd, none ditto HWs, SWchar, SWline, none ditto 0... ±999999 3.2.2.50. 57 3.2 Remote control commands &SmplData Object Description Input range Reference & Root : ├ SmplData Sample data : ├ .Status Status of silo memory ├ .OFFSilo Current sample data │ ├ .Id1 Sample identification 1 │ ├ .Id2 Sample identification 2 │ ├ .Id3 Sample identification 3 │ ├ .ValSmpl Sample size │ ├ .UnitSmpl Unit of sample size ├ .ONSiloCurrent sample data │ ├ .Counter Counter of silo memory │ │ ├ .MaxLines Maximum lines │ │ ├ .FirstLine First line │ │ ├ .LastLine Last line │ ├ .EditLine Editing silo lines │ │ ├ .1 1st silo line │ │ │ ├ .Method Method name │ │ │ ├ .Id1 Sample identification 1 │ │ │ ├ .Id2 Sample identification 2 │ │ │ ├ .Id3 Sample identification 3 │ │ │ ├ .ValSmpl Sample size │ │ │ ├ .UnitSmpl Unit of sample size │ │ │ ├ .C24 Value of variable C24 │ │ │ ├ .C25 Value of variable C25 │ │ │ ├ .Mark Mark of silo line │ │ ├ up to 255 lines │ ├ .DelLine Delete silo line │ │ ├ .LineNum Line number │ ├ .DelAll Delete silo line │ ├ .CycleLines Cycle lines │ ├ .SaveLines Save results 58 ON, OFF 3.2.2.51. up to 8 ASCII char up to 8 ASCII char up to 8 ASCII char ±X.XXXXX up to 5 ASCII char 3.2.2.52. ditto ditto ditto ditto read only read only read only 3.2.2.53. ditto ditto up to 8 ASCII char up to 8 ASCII char up to 8 ASCII char up to 8 ASCII char ±X.XXXXX up to 5 ASCII char read only read only read only 3.2.2.54. ditto ditto ditto ditto ditto ditto ditto ditto $G 1...255, OFF $G ON, OFF ON, OFF 3.2.2.55. ditto 3.2.2.56. 3.2.2.57. 3.2.2.58. 795 KFT Titrino 3.2 Remote control commands &HotKey Object Description Input range Reference & Root : ├ HotKey : ├ .User │ ├ .Name │ ├ .Delete │ │ ├ .Name │ ├ .DelAll │ ├ .List │ │ ├ .1 │ │ │ ├ .Name │ │ ├ up to 99 795 KFT Titrino Keys with direct access User name Input of user name Delete user Input of user name Delete all users List of users User 1 Name of user up to 10 ASCII char $G up to 10 ASCII char $G read only 3.2.2.59. ditto ditto ditto ditto ditto 59 3.2 Remote control commands &Info Object Description Input range Reference & Root : ├ Info Current data : ├ .Report Transmission of formatted reports │ ├ .Select Report type │ │ │ │ │ │ ├ .Checksums Checksums │ ├ .MPList Checksum of meas.point list │ ├ .ActualMethod Checksum of current method │ ├ .DetermData Determination data │ ├ .Write Read/write for several nods │ ├ .ExV Volume of Exchange/Dosing unit │ ├ .MPList Measuring point list │ │ ├ .1 Measuring point 1 │ │ │ ├ .Attribute Attribute │ │ │ ├ .X X coordinate │ │ │ ├ .Y Y coordinate │ │ │ ├ .Z1 Z1 coordinate │ │ │ ├ .Z2 Z2 coordinate │ │ │ for each measuring point │ ├ .TitrResults Titration results │ ├ .RS Calculated results │ │ ├ .1 1st result │ │ │ ├ .Value Value │ │ ├ up to 9 results │ ├ .EP Endpoint │ │ ├ .1 1st result │ │ │ ├ .V Value │ │ │ ├ .Meas Measured value │ │ │ ├ .Mark without meaning │ │ ├ up to 9 EP's │ ├ .Var Variables C4X │ │ ├ .C40 Start measured value │ │ ├ .C41 Titration end volume │ │ ├ .C42 Titration time │ │ ├ .C43 Volume drift │ │ ├ .C44 Titration temperature │ │ ├ .C45 Start volume │ │ ├ .DTime Time for drift corr.or dosing time 60 $G 3.2.2.60. configuration, parameters, smpl data, statistics, silo, C-fmla, def, user method, full, short, mplist, curve, scalc full, scalc srt, calc, all, ff ditto $G read only read only 3.2.2.61. ditto ditto $G ON, OFF read only/read+write 3.2.2.62. read only/read+write read only/read+write read only/read+write read only/read+write read only/read+write ditto ditto ditto ditto ditto ditto read only 3.2.2.63. read only read only ditto read only/read+write read only/read+write read only/read+write read only/read+write read only/read+write read only/read+write read only/read+write ditto 795 KFT Titrino 3.2 Remote control commands "Info", continuation ├ .StatisticsVal Statistics values │ ├ .ActN Number of results in chart │ ├ .1 1st mean │ │ ├ .Mean Mean │ │ ├ .Std Absolute standard deviation │ │ ├ .RelStd Relative standard deviation │ ├ up to 9 mean values │ ├ .SiloCalc Values of silo calculations │ ├ .C24 Values of variable C24 │ │ ├ .Name Name │ │ ├ .Value Value │ │ ├ .Unit Unit │ ├ .C25 as for C24 │ ├ .C26 Values of variable C26 │ │ ├ .ActN Number of single values │ │ ├ .Mean Mean value │ │ ├ .Std Absolute standard deviation │ │ ├ .RelStd Relative standard deviation │ ├ .C27 as for C26 │ ├ .ActualInfo Current data │ ├ .Inputs I/O Inputs │ │ ├ .Status Line status │ │ ├ .Change Change of line status │ │ ├ .Clear Clear change │ ├ .Outputs as for I/O Inputs │ ├ .Assembly From Assembly │ │ ├ .CyclNo Cycle number │ │ ├ .Counter Assembly counter │ │ │ ├ .V Volume counter │ │ │ ├ .Clear Clears counter │ │ ├ .Meas Measured value │ ├ .Titrator From Titrator │ │ ├ .CyclNo Cycle number │ │ ├ .V Volume │ │ ├ .Meas Measured indicator voltage │ │ ├ .dVdt Volume drift dV/dt │ │ ├ .dMeasdt Measured value drift │ │ ├ .dMeasdV 1st deviation of titration curve │ ├ .MeasPt Entry in measuring point list │ │ ├ .Index Index of entry │ │ ├ .X X coordinate │ │ ├ .Y Y coordinate │ │ ├ .Z1 Z1 coordinate │ │ ├ .Z2 Z2 coordinate │ ├ .EP EP entry │ │ ├ .Index Index of entry │ │ ├ .X X coordinate │ │ ├ .Y Y coordinate 795 KFT Titrino read only 3.2.2.64. read only read only read only ditto ditto ditto read only read only read only 3.2.2.65. ditto ditto read only read only read only read only ditto ditto ditto ditto read only read only $G 3.2.2.66. ditto ditto read only read only read only $G read only 3.2.2.67. 3.2.2.68. ditto ditto 3.2.2.69. read only read only read only read only read only read only 3.2.2.70. ditto ditto ditto ditto ditto read only read only read only read only read only 3.2.2.71. ditto ditto ditto ditto read only read only read only ditto ditto ditto 61 3.2 Remote control commands │ ├ .Oven │ │ ├ .HeatTime │ │ ├ .SampleTemp │ │ ├ .LowTemp │ │ ├ .HighTemp │ │ ├ .GasFlow │ │ ├ .UnitFlow │ ├ .Display │ │ ├ .L1 │ │ ├ up to line 8 │ │ ├ .DelAll │ ├ .Comport │ │ ├ .Number │ ├ .Assembly │ ├ CycleTime │ ├ ExV 62 "Info", continuation Oven data Heating time Sample temperature Lowest temperature Highest temperature Gas flow Unit of gas flow Display Text line 1 Delete display Comport COM where PC is connected Assembly Cycle time Volume of Exchange/Dosing unit read only read only read only read only read only read only 3.2.2.72. ditto ditto ditto ditto ditto up to 32 ASCII char 3.2.2.73. $G ditto read only 3.2.2.74. read only read only 3.2.2.75. ditto 795 KFT Titrino 3.2 Remote control commands &Assembly Object Description Input range Reference & Root : ├ Assembly ├ . Bur │ ├ .Rates │ │ ├ .Forward │ │ │ ├ .Select │ │ │ ├ .Digital │ │ ├ .Reverse │ │ │ ├ .Select │ │ │ ├ .Digital │ ├ .Fill │ ├ .ModeDis │ │ ├ .Select │ │ ├ .V │ │ ├ .Time │ │ ├ .VStop │ │ ├ .AutoFill │ ├ .Meas │ ├ .Status │ ├ .MeasInput │ ├ .Ipol │ ├ .Upol │ ├ .Outputs │ ├ .AutoEOD │ ├ .SetLines │ │ ├ .L0 │ │ ├ up to L13 │ ├ .ResetLines │ ├ .Stirrer │ 795 KFT Titrino Assembly control Buret Rates Forward rate Type of rate control Digital rate as for forward rate Type of rate control Digital rate Fill Dispensing Type of dispensing control Volume to be dispensed Time to dispense Limit volume Filling after each increment digital, analog 0...150, max. 3.2.2.76. ditto digital, analog 0...150, max. $G,$H,$C $G,$S,$H,$C volume, time 0.0001...0.1...9999 0.25...1...86 400 0.0001...9999, OFF ON, OFF ditto ditto 3.2.2.77. 3.2.2.78. ditto ditto ditto ditto ditto Measuring Measuring ON/OFF Selection of measuring input Polarization current Polarization voltage ON, OFF Ipol, Upol 0...1...±127 0...400...±1270 3.2.2.79. ditto ditto ditto I/O outputs Automatic output of EOD Set I/O lines Signal on L0 ON, OFF 3.2.2.80. $G ditto active,inactive,pulse,OFF ditto Reset I/O lines $G Stirrer ON, OFF ditto 3.2.2.81. 63 3.2 Remote control commands &Setup Object Description Input range Reference & Root : ├ Setup ├ .Comport ├ .Keycode ├ .Tree │ ├ .Short │ ├ .ChangedOnly │ ├ .Trace │ ├ .Lock │ ├ .Keyboard │ ├ .Config │ ├ .Parameter │ ├ .SmplData │ ├ .UserMeth │ │ ├ .Recall │ │ ├ .Store │ │ ├ .Delete │ └ .Display │ ├ .Mode │ ├ .StartWait │ ├ .FinWait │ ├ .SendMeas │ ├ .SendStatus │ ├ .Interval │ │ ├ .Select │ ├ .Assembly │ │ ├ .CyclNo │ │ ├ .V │ │ ├ .Meas │ ├ .Titrator │ │ ├ .CyclNo │ │ ├ .V │ │ ├ .Meas │ │ ├ .dVdt │ │ ├ .dMeasdt │ │ ├ .dMeasdV │ 64 Settings for the operating mode Output of automatic info Send key code Sending format of path info Short format of path Paths of modified nodes only Message on changed values Lock key functions Lock all keyboard keys Lock <CONFIG> key Lock <PARAM> key Lock <SMPL DATA> key Lock functions Lock “loading” Lock “saving” Lock “deletion” Lock display function Setting waiting intervals Waiting time after start Waiting time after run 1,2,1&2 ON, OFF 3.2.2.82. 3.2.2.83. ON, OFF ON, OFF 3.2.2.84. ditto ON, OFF 3.2.2.85. ON, OFF ON, OFF ON, OFF ON, OFF 3.2.2.86. ditto ditto ditto ON, OFF ON, OFF ON, OFF ON, OFF ditto ditto ditto ditto ON, OFF ON, OFF 3.2.2.87. ditto Automatic sending of measured values Connect/disconnect sending ON, OFF Time interval 0.08...4...16200, MPList Selection Assembly, Titrator From assembly Cycle number ON, OFF Volume ON, OFF Measured indicator voltage ON, OFF From Titrator Cycle number ON, OFF Volume ON, OFF Measured indicator voltage ON, OFF Volume drift dV/dt ON, OFF Measured value drift ON, OFF 1st deviation of titration curve ON, OFF 3.2.2.88. ditto 3.2.2.89. 3.2.2.90. ditto ditto 3.2.2.91. ditto ditto ditto ditto ditto 795 KFT Titrino 3.2 Remote control commands ├ .AutoInfo │ ├ .Status │ ├ .P │ ├ .T │ │ ├ .R │ │ ├ .G │ │ ├ .GC │ │ ├ .S │ │ ├ .B │ │ ├ .F │ │ ├ .E │ │ ├ .H │ │ ├ .C │ │ ├ .O │ │ ├ .N │ │ ├ .Re │ │ ├ .Si │ │ ├ .M │ │ ├ .EP │ │ ├ .RC │ ├ .C │ │ ├ .B1 │ │ ├ .R1 │ │ ├ .B2 │ │ ├ .R2 │ ├ .I │ ├ .O │ ├ .Graphics │ ├ .Grid │ ├ .Frame │ ├ .Scale │ ├ .Recorder │ │ ├ .Right │ │ ├ .Feed │ ├ .PowerOn ├ .Initialise │ ├ .Select │ ├ .RamInit ├ .InstrNo ├ .Value 795 KFT Titrino "Setup", continuation Automatic message for changes Switch AutoInfo on/off When mains is switched on Titrator infos When "ready" When method started When start is initiated When stopped Begin of method End of process Error When "hold" Continue after "hold" Conditioning OK Conditioning not OK Request after start Silo empty Entry in measuring point list Entry in EP list Recalculation of results done Comport infos When COM1 sends a report When COM1 is ready again When COM2 sends a report When COM2 is ready again Changing an I/O input Changing an I/O output Changing the curve output Grid on curve Frame on curve Type of depending axis Length of axes Length of meas value axis Length of paper drive axis RESET (power on) Set default values Selection of branch Initialization of working mem. Device Identification Input of device identification ON, OFF ON, OFF 3.2.2.92. ditto ditto ON, OFF ON, OFF ON, OFF ON, OFF ON, OFF ON, OFF ON, OFF ON, OFF ON, OFF ON, OFF ON, OFF ON, OFF ON, OFF ON, OFF ON, OFF ON, OFF ditto ditto ditto ditto ditto ditto ditto ditto ditto ditto ditto ditto ditto ditto ditto ditto ON, OFF ON, OFF ON, OFF ON, OFF ON, OFF ON, OFF ditto ditto ditto ditto ditto ditto ON, OFF ON, OFF Full, Auto 0.2...0.5...1.00 0.01...0.05...1.00 $G $G ActMeth,Config,Silo, Assembly,Setup,All $G $G 8 ASCII characters 3.2.2.93. ditto ditto ditto ditto 3.2.2.94. 3.2.2.95. ditto 3.2.2.96. 3.2.2.97. ditto 65 3.2 Remote control commands &Diagnose Object Description Input range Diagnose Output of adjustment parameters $G Reference & Root : ├ Diagnose ├ .Report 66 3.2.2.98. 795 KFT Titrino 3.2 Remote control commands 3.2.2 Description of the remote control commands 3.2.2.1. Mode $G, $S, $H, $C Start and stop ($G, $S) or hold of the current method (3.2.2.3) with $H and continue with $C. $G also serves to continue after inquiries of identifications and sample size after the start (see 3.2.2.26). 3.2.2.2. Mode.QuickMeas $G, $S Start and stop of a measurement in the basic mode with the parameters (measured quantity, measuring input) of the current method. Corresponds to the <meas/hold> key. With an ongoing measurement, the current mode can be started. This stops the measurement automatically. 3.2.2.3. Mode.Select KFT Mode.KFTQuantity Ipol, Upol Selection of the standard mode. Mode and the measured quantity belong to the complete selection. If a method is selected from the method memory, the nodes &Mode.Select and &Mode.XXXQuantity are overwritten with mode and measured quantity of the corresponding user method. 3.2.2.4. Mode.Name read only Name of the current method in the working memory. $Q sends 8 ASCII characters. Standard methods carry the name ********. The node can be set read + write, see 3.2.2.62. 3.2.2.5. Mode.Def.Formulas.1.Formula EPX, CXX, RSX, +, –, ∗, /, (, ) Mode.Def.Formulas.1.TextRS up to 8 ASCII characters Mode.Def.Formulas.1.Decimal 0...2...5 Mode.Def.Formulas.1.Unit up to 6 ASCII characters Mode.Def.Formulas.1.Limits ON, OFF Mode.Def.Formulas.1.LoLim 0...±999 999 Mode.Def.Formulas.1.UpLim 0...±999 999 Mode.Def.Formulas.1.Output active, pulse, OFF Mode.Def.Formulas.2.Formula etc. up to .9 Entry of formulas. Rules for formula entry, see page 25. Example: "(EP2–EP1)∗C01/C00" In addition to the formula, a text for result output, the number of decimal places and a unit for the result output can be selected. "No unit" is selected with the blank string. In place of "RSX", a result name may be entered (.TextRS). This name is outputted in the report full, short, scalc full and scalc srt. It is used for the result and the corresponding mean value. 795 KFT Titrino 67 3.2 Remote control commands The limit control for results can also be activated. If a result is out of limit, a message appears in the result report, E196 is sent, and output line L13 can be set. 3.2.2.6. Mode.Def.SiloCalc.Assign.C24 RSX, EPX, CXX Mode.Def.SiloCalc.Assign.C25 RSX, EPX, CXX Mode.Def.SiloCalc.MatchId id1, id1&2, all, OFF .Assign.C2X: Assignment to store results in the silo as C2X. .MatchId: Indication which sample identification(s) have to match so that the results can be combined. 3.2.2.7. Mode.Def.ComVar.C30 RSX, MNX, EPX, CXX Mode.Def.ComVar.C31 etc., up to .C39 Assignment of common variables. The values of the common variables are to be found in &Config.ComVar. They can be viewed and entered there, see 3.2.2.50. 3.2.2.8. Mode.Def.Report.Assign1 Mode.Def.Report.Assign2 param, full, short, mplist, curve, scalc full, scalc srt, calc, ff Definition of the report sequence, which is outputted automatically at the end of the determination. Entries of more than one block have to be separated with ";". .Assign1: Output to COM1 of the Titrino. Identical for COM2. 3.2.2.9. Mode.Def.Mean.1.Assign RS1, RSX, EPX, CXX Mode.Def.Mean.2.Assign etc., up to .9 Assignment of the statistics calculations. Valid assignments are a requirement for statistics calculations. In addition, the statistics calculation must be switched on, see 3.2.2.24. Rules for statistics calculations see page 29. 3.2.2.10. Mode.CFmla Mode.CFmla.1.Value 0...±999999 Mode.CFmla.2.Value etc., up to .19 Calculation constants specific to a method. Stored in the method memory of the Titrino. Operands specific to the sample (3.2.2.52 and 3.2.2.63) and values of common variables (3.2.2.50) on the other hand are not stored with the methods. 68 795 KFT Titrino 3.2 Remote control commands 3.2.2.11. Mode.Parameter.CtrlPara.EP Ipol: Upol: 0...250...±2000 0...25...±200.0 Mode.Parameter.CtrlPara.UnitEp read only Setting of the EP, resp. Control point in mV (with Ipol) or µA (with Upol). The corresponding unit can be read with .UnitEP. 3.2.2.12. Mode.Parameter.CtrlPara.Dyn Ipol: Upol: 1...100...2000 0.1...10...200.0 read only 0.01...10...150, max. 0.1...9.9, min. Mode.Parameter.CtrlPara.UnitDyn Mode.Parameter.CtrlPara.MaxRate Mode.Parameter.CtrlPara.MinIncr Control parameters. .Dyn: Dynamics (control range) in mV (with Ipol) or µA (with Upol). The corresponding unit can be read with .UnitDyn. .MaxRate: Maximum allowed titration rate in mL/min. Max. means maximum possible rate with mounted Exchange Unit. .MinIncr: Minimum volume increment in µL. OFF means that the criterion is not monitored. 3.2.2.13. Mode.Parameter.CtrlPara.Stop.Type drift, time Mode.Parameter.CtrlPara.Stop.Drift 1...20...999 Mode.Parameter.CtrlPara.Stop.Time 0...10...999, inf. Mode.Parameter.CtrlPara.Stop.StopT 0...99999, OFF Type and size of the stop criterion of the titration. .Type: Type of stop criterion after stop drift or switch-off delay time. .Drift: Stop drift in µL/min. Applies when "drift" has been selected. .Time: Switch-off delay time in s. Applies when "time" has been selected. "inf." means infinite. .StopT: Stop time in s. Applies when "time" has been selected and the value of .Time is set to "inf.". 3.2.2.14. Mode.Parameter.TitrPara.Direction +, –, auto Titration direction. "auto" means the titration direction is determined automatically by the instrument. 3.2.2.15. Mode.Parameter.TitrPara.XPause Pause time in s. Runs before dosing the start volume. 795 KFT Titrino 0...999999 69 3.2 Remote control commands 3.2.2.16. Mode.Parameter.TitrPara.StartV.Type abs., rel., OFF Mode.Parameter.TitrPara.StartV.V 0...999.99 Mode.Parameter.TitrPara.StartV.Factor 0...±999999 Mode.Parameter.TitrPara.StartV.Rate 0.01...150, max. Start volume. If an absolute start volume (abs.) has been selected, the volume in mL is valid. A relative start volume (rel.) is dispensed as a function of the sample size: Start volume in mL = smpl size ∗ factor The factor is valid. The dispensing rate in mL/min applies to both cases. Max. means maximum possible dispensing rate with the Exchange Unit in current use. 3.2.2.17. Mode.Parameter.TitrPara.Pause 0...999999 Pause time in s. Is waited off after the dispensing of the start volume. 3.2.2.18. Mode.Parameter.TitrPara.ExtrT Extraction time in s. 0...999999 3.2.2.19. Mode.Parameter.TitrPara.Ipol –127...50...+127 Mode.Parameter.TitrPara.Upol –1270...400...+1270 Mode.Parameter.TitrPara.PolElectrTest ON, OFF With Ipol, the inquiries for the polarization current in µA (Ipol) and .PolElectrTest are valid. With Upol, the inquiry for the polarization voltage in mV (Upol) is valid. Entry in steps of 10 mV. Besides .PolElectrTest is valid. If the test for polarized electrodes is switched on, it is performed on changeover from the inactive state to an active state (titration or conditioning). 3.2.2.20. Mode.Parameter.TitrPara.Temp Titration temperature in °C. –170.0...25.0...500.0 3.2.2.21. Mode.Parameter.TitrPara.TDelta 1...2...999999 Time interval in s for the entry of a measurement point in the list of measured points. 70 795 KFT Titrino 3.2 Remote control commands 3.2.2.22. Mode.Parameter.StopCond.VStop.Type abs., rel., OFF Mode.Parameter.StopCond.VStop.V 0...99.99...9999.99 Mode.Parameter.StopCond.VStop.Factor 0...±999999 Stop volume. If an absolute stop volume (abs.) has been selected, the volume in mL is valid. A relative stop volume (rel.) is dispensed as a function of the sample size: Stop volume in mL = smpl size ∗ factor The factor is valid. OFF means that the criterion is not monitored. 3.2.2.23. Mode.Parameter.StopCond.FillRate 0.01...150, max. Filling rate in the titration in mL/min. Max. means maximum possible filling rate with the Exchange Unit in current use. 3.2.2.24. Mode.Parameter.Statistics.Status Mode.Parameter.Statistics.MeanN Mode.Parameter.Statistics.ResTab.Selected ON, OFF 2...20 original, delete n, delete all 1...20 Mode.Parameter.Statistics.ResTab.DelN Entries for the statistics calculations. .Status: On/off switching. Requirement for statistics calculations is a valid assignment, see 3.2.2.9. .MeanN: Number of individual results for statistics calculations. .ResTab.Select: Selection of the table for the statistics calculations. original: Original table. The original table is (again) set up, i.e. any individual results which have been deleted are reincorporated in the statistics calculations. delete n: Single result lines are removed from the statistics calculation. All results of the corresponding line in the statistics table are deleted. Specification of the line number in .ResTab.DelN. delete all: Clear entire statistics table. The results can not be reactivated. .ResTab.DelN: Specification of the line number to be deleted. 3.2.2.25. Mode.Parameter.Presel.Cond ON, OFF Mode.Parameter.Presel.DriftDisp ON, OFF Mode.Parameter.Presel.DCor.Type auto, man., OFF Mode.Parameter.Presel.DCor.Value 0.0...99.9 .Cond: Conditioning ON/OFF .DriftDisp: Drift display during conditioning ON/OFF. .DCor.Type: Type of drift take-over for the drift correction. auto: Take-over of the drift value at start. .DCor.Value: Drift value for the manual drift correction. 795 KFT Titrino 71 3.2 Remote control commands 3.2.2.26. Mode.Parameter.Presel.IReq id1, id1&2, all, OFF Mode.Parameter.Presel.SReq value, unit, all, OFF Automatic inquiry after the start of the determination. From such an inquiry, the determination continues if the requested entry/entries is/are made, e.g. &SmplData.OFFSilo.Id1 (see 3.2.2.52) or with &M $G, see 3.2.2.1. $H is not possible in requests. 3.2.2.27. Mode.Parameter.Presel.LimSmplSize.Status Mode.Parameter.Presel.LimSmplSize.LoLim Mode.Parameter.Presel.LimSmplSize.UpLim Limit control for the sample size. ON, OFF 0.0...999 999 0.0...999 999 3.2.2.28. Mode.Parameter.Presel.Oven COM1, COM2, no If an oven is connected, its result will be incorporated into the result report of the Titrino. If there is no oven connected via RS232, the setting of this parameter has to be "no". 3.2.2.29. Mode.Parameter.Presel.ActPuls first, all, cond., OFF Output of a pulse on the I/O line "Activate", see page 126. 3.2.2.30. UserMeth.FreeMem read only Memory space, available for user methods or silo lines. $Q sends the number of free bytes, e.g. "4928". 3.2.2.31. UserMeth.Recall $G UserMeth.Recall.Name up to 8 ASCII characters UserMeth.Store $G UserMeth.Store.Name up to 8 ASCII characters UserMeth.Delete $G UserMeth.Delete.Name up to 8 ASCII characters UserMeth.DelAll $G Management of the internal method memory: Load, store and delete methods. An action is performed if "$G" is sent to the corresponding node just after entering the name. Do not use blank characters before and after method name! .DelAll: Deletes all methods in the user memory. 72 795 KFT Titrino 3.2 Remote control commands 3.2.2.32. UserMeth.List.1.Name read only UserMeth.List.1.Mode read only UserMeth.List.1.Quantity read only UserMeth.List.1.DosUnit read only UserMeth.List.1.Bytes read only UserMeth.List.1.Checksum read only for each method List of the methods in the user method memory with the following characteristics: .Name: Name of the method .Mode: Mode .Quantity: Measured quantity .DosUnit: Buret of the method .Bytes: Number of bytes of the user memory used by the method .Checksum: Checksum of the method, see 3.2.2.61. 3.2.2.33. Config.Monitoring.Validation.Status Config.Monitoring.Validation.Interval Config.Monitoring.Validation.Counter Config.Monitoring.Validation.ClearCount Monitoring of validation. .Interval: Time interval in days for validation. .Counter: Time counter in days since last validation. .ClearCount: Clears the above counter. ON, OFF 1...365...9999 0...9999 $G 3.2.2.34. ON, OFF YYYY-MM-DD Config.Monitoring.Service.Status Config.Monitoring.Service.Date Monitoring of service interval. 3.2.2.35. Config.Monitoring.DiagRep Printing of system test report after each switching on of the Titrino. ON, OFF 3.2.2.36. Config.PeriphUnit.CharSet1 Epson, Seiko, Citizen, HP, IBM Config.PeriphUnit.CharSet2 Selection of the character set and the graphics control characters for COM1 resp. COM2 of the Titrino. IBM means the IBM character set following character set table 437 and IBM graphics control characters. Select 'IBM' for work with the computer. 3.2.2.37. Config.PeriphUnit.RepToComport 1, 2, 1&2 Selection of COM of the Titrino where manually triggered reports should be outputted. 3.2.2.38. Config.PeriphUnit.Balance Selection of the balance type. 795 KFT Titrino Sartorius,Mettler,Mettler AT, AND,Precisa 73 3.2 Remote control commands 3.2.2.39. Config.PeriphUnit.Stirrer ON, OFF Automatic stirrer control. With "ON" the stirrer will be switched on after starting a method. At the end of the method it is switched off again. 3.2.2.40. Config.PeriphUnit.RemoteBox.Status Config.PeriphUnit.RemoteBox.Keyboard Config.PeriphUnit.RemoteBox.Barcode ON, OFF US, deutsch, francais, español, schweiz. input, method, id1, id2, id3, smpl size Connections via Remote Box. .Status: Select if a Remote Box is connected. .Keyboard: Type of keyboard which is connected to the Remote Box. .Barcode: Select target in Titrino where you wish to have the string from the barcode reader. "input" means that the string comes into the field where the cursor is currently placed. 3.2.2.41. Config.Aux.Language Selection of the dialog language. english, deutsch, francais, español, italiano, portugese, svenska 3.2.2.42. Config.Aux.Set $G Config.Aux.Set.Date YYYY-MM-DD Config.Aux.Set.Time hh:mm Date and time. Input format of the date: Year-month-day, two-digit, enter leading zeros. Input format for the time: Hours:minutes, two-digit, enter leading zeros. Date and time have to be set with &Config.Aux.Set $G just after entry of the value. 3.2.2.43. Config.Aux.RunNo 0...9999 Current sample number. Set to 0 on power on and initialization. After 9999, counting starts again at 0. 3.2.2.44. Config.Aux.AutoStart Number of automatic, internal starts. 1...9999, OFF 3.2.2.45. Config.Aux.StartDelay 0...999999 Start delay time in s. During this time, the data of the preceding determination are retained. 3.2.2.46. Config.Aux.ResDisplay bold, standard Character set for the result display at the end of the determination. 74 795 KFT Titrino 3.2 Remote control commands 3.2.2.47. Config.Aux.DevName up to 8 ASCII characters Name of the instrument for connections with several units. It is advisable to use only the letters A...Z (ASCII No. 65...90), a...z (ASCII No. 97...122) and the numbers 0...9 (ASCII No. 48...57) when the function Setup.AutoInfo (3.2.2.92) is used at the same time. If a name has been entered, it will be printed out in the result report (full, short). 3.2.2.48. Config.Aux.Prog Output of the program version. The Titrino sends "795.0010" on requests with $Q. 3.2.2.49. read only Config.RSSet1 Config.RSSet1.Baud $G 300, 600, 1200, 2400, 4800, 9600, 19200, 38400, 57600, 115200 Config.RSSet1.DataBit 7, 8 Config.RSSet1.StopBit 1, 2 Config.RSSet1.Parity even, odd, none Config.RSSet1.Handsh HWs, SWchar, SWline, none $G sets all RS settings. The changes are performed only if the instrument is inactive. After the setting of the interface parameters, wait at least 2 s to allow the components to equilibrate. Settings of the values for the data transmission via the RS interface: baud rate, data bit, stop bit, parity and type of handshake, see also page 90ff. Baud rates >9600 need a PC which is equipped accordingly (e.g. with 16550 component). The setting of the values must be initiated with $G immediately after entry of the values. 3.2.2.50. Config.ComVar.C30 with up to .C39, etc. 0... ±999999 Values of the common variables from C30 up to C39. Insert the common variables directly or describe the determination results directly from the method, see 3.2.2.7. 3.2.2.51. SmplData.Status ON, OFF On/off switching of silo memory. When the silo memory is switched on, the sample data are fetched from the lowest valid silo line. 795 KFT Titrino 75 3.2 Remote control commands 3.2.2.52. SmplData.OFFSilo.Id1 up to 8 ASCII characters SmplData.OFFSilo.Id2 up to 8 ASCII characters SmplData.OFFSilo.Id3 up to 8 ASCII characters SmplData.OFFSilo.ValSmpl 6-digits, sign and decimal point SmplData.OFFSilo.UnitSmpl up to 5 ASCII characters Current sample data. The identifications Id1...Id3 can be used in formulas as sample-specific calculation constants C21...C23. If "no unit" is desired for the unit of the sample size, the blank string must be entered. 3.2.2.53. SmplData.ONSilo.Counter.MaxLines SmplData.ONSilo.Counter.FirstLine SmplData.ONSilo.Counter.LastLine Information on silo memory. .MaxLines: Maximum possible number of silo lines. .FirstLine: Lowest valid silo line. .LastLine: Last occupied silo line. read only read only read only 3.2.2.54. SmplData.ONSilo.EditLine.1.Method up to 8 ASCII characters SmplData.ONSilo.EditLine.1.Id1 up to 8 ASCII characters SmplData.ONSilo.EditLine.1.Id2 up to 8 ASCII characters SmplData.ONSilo.EditLine.1.Id3 up to 8 ASCII characters SmplData.ONSilo.EditLine.1.ValSmpl 6-digits, sign and dec.point SmplData.ONSilo.EditLine.1.UnitSmpl up to 5 ASCII characters SmplData.ONSilo.EditLine.1.C24 read only SmplData.ONSilo.EditLine.1.C25 read only SmplData.ONSilo.EditLine.1.Mark read only etc., up to .255 Contents of a silo line. .Method: Method used to process the sample, from the method memory or from the card. .Id: The identifications Id1...Id3 can also be used as sample-specific calculation constants C21...C23 in formulas. .UnitSmpl: If "no unit" is desired for the sample size, the blank string must be entered. .C24, .C25: Results which have been assigned to C24 and C25. .Mark: Mark of the silo line: "∗"=deleted line, "+"=line which is worked off, "–"= line which is worked off and not valid for silo calculations (deleted), "/" last worked-off line, where recalculation can still be done. Silo lines which have been worked off are "read only". 3.2.2.55. SmplData.ONSilo.DelLine $G SmplData.ONSilo.DelLine.LineNum 1...255, OFF Deletion of a silo line. The line # is deleted with &SmplData.ONSilo.DelLine $G. If a formerly deleted line is edited again, it becomes valid (function "undelete"). 76 795 KFT Titrino 3.2 Remote control commands 3.2.2.56. SmplData.ONSilo.DelAll Deletes the entire silo memory. Must be triggered with $G. $G 3.2.2.57. SmplData.ONSilo.CycleLines ON, OFF Silo data cycling. With "ON", executed lines are copied to the next free silo lines, see page 40. Exercise caution if you edit the silo memory during the determinations! 3.2.2.58. SmplData.ONSilo.SaveLines ON, OFF Silo lines are not deleted when they are worked off. Assigned results are stored as C24 and C25. "Save lines" can only be set to "ON" if the silo is completely empty. Delete the silo, see 3.2.2.56. 3.2.2.59. HotKey.User.Name up to 10 ASCII characters HotKey.User.Delete $G HotKey.User.Delete.Name up to 10 ASCII characters HotKey.User.DelAll $G HotKey.User.List.1.Name read only Management of user names. .Name: Input of user names. .Delete.Name: Deletes selected user name with &HotKey.User.Delete $G. .List: List of all user names. 3.2.2.60. $G configuration, parameters, smpl data, statistics, silo, C-fmla, def, user method, full, short, mplist, curve, scalc full, scalc srt, calc, all, ff $G sends the selected report to the COM which is set in &Config.PeriphUnit.RepToComport: configuration: Configuration report. Is not accessible during a running determination. parameters: Parameter report of the current method. During a running determination only "live"-parameters are accessible. smpl data: Current sample data. statistics: Statistics table with the individual results. silo: Contents of the silo memory. C-fmla: Contents of the <C-fmla> key. def: Contents of the <def> key. user method: Contents of the method memory. full: Full result report of the last completed determination. short: Short result report of the last completed determination. mplist: Measuring point list of the running determination. curve: Curve volume vs. time of the last determination. scalc full: Full report of the silo calculations. scalc srt: Short report of the silo calculations. calc: Calculation report of the current method. all: All reports. ff: Form feed on printer. 795 KFT Titrino Info.Report Info.Report.Select 77 3.2 Remote control commands Reports which are sent from the Titrino are marked with space (ASCII 32) and ' at the beginning. Then an individual identifier for each report follows. Reports which are triggered by RS232 ($G) have the same introducer but without preceding space, i.e. they start with '. 3.2.2.61. Info.Checksums $G Info.Checksums.MPList read only Info.Checksums.ActualMethod read only The checksums can be used to identify the content of a file unequivocally, e.g. files with identical content have identical results of the checksums. An empty file has checksum "0". The calculation of the checksums is triggered with $G. .MPList: Result of the checksum of the current measuring point list. .ActualMethod: Result of the checksum of the current method in the working memory. Identical methods with different method names have the same results of the checksum. 3.2.2.62. Info.DetermData $G Info.DetermData.Write ON, OFF Info.DetermData.MPList.1.Attribute read only/read+write Info.DetermData.ExV read only/read+write Info.DetermData.MPList.1.X read only/read+write Info.DetermData.MPList.1.Y read only/read+write Info.DetermData.MPList.1.Z1 read only/read+write Info.DetermData.MPList.1.Z2 read only/read+write for every measuring point Determination data in hexadecimal format. A measuring point list is available. Recalculation of the measuring data is triggered with $G. .Write: With "ON", the following nodes can be overwritten: &Info.DetermData.MP.List, &Info.TitrResults.Var.C4X (X = 0...5), and &Mode.Name. .ExV: Volume of the exchange unit, with which the determination was executed .MPList.1.Attribute: Attribute .MPList.X: X coordinate, time .MPList.Y: Y coordinate, volume .MPList.Z1: Z1 coordinate, measuring value .MPList.Z2: without meaning 78 795 KFT Titrino 3.2 Remote control commands 3.2.2.63. Info.TitrResults.RS.1.Value read only etc., up to .9 Info.TitrResults.EP.1.V read only Info.TitrResults.EP.1.Meas read only etc., up to .2 Info.TitrResults.Var.C40 read only/read+write etc., up to .C45 Info.TitrResults.Var.DTime read only/read+write .RS: Values of the calculated results. .EP: Endpoints: Volume coordinate in mL, e.g. "1.2340" Measured value coordinate in mV (with Ipol) "–241" or µA (with Upol) "43.7". .Var: Various variables. You may overwrite the variables C40...C45, see 3.2.2.62. C40: Initial measured value in mV (with Ipol) "41" or µA (with Upol). C41: End volume in mL, "12.5360". C42: Time from start of titration to end in s, "62". C43: Volume drift on start of KFT titration from the conditioning in µL/min, "3.5". C44: Temperature in °C. C45: Start volume in mL, "2.800". DTime: Time for the drift correction in KFT with conditioning. 3.2.2.64. Info.StatisticsVal.ActN Info.Statistics.1.Mean Info.Statistics.1.Std Info.Statistics.1.RelStd etc. up to .9 The current values of the statistics calculation. $Q sends, e.g. ActN: Current value of the individual results Data for MN1: Mean: Mean value (decimal places as in result) Std: Standard deviation (1 decimal place more than in result) RelStd: Relative standard deviation (in %, 2 decimal places) read only read only read only read only "3" "3.421" "0.0231" "0.14" 3.2.2.65. Info.SiloCalc.C24.Name read only Info.SiloCalc.C24.Value read only Info.SiloCalc.C24.Unit read only for .C25 as for .C24 Info.SiloCalc.C26.ActN read only Info.SiloCalc.C26.Mean read only Info.SiloCalc.C26.Std read only Info.SiloCalc.C26.RelStd read only for .C27 as for .C26 The current values from the silo calculations. C26 is the mean value out of the C24 variables; C27 comes from C25. 795 KFT Titrino 79 3.2 Remote control commands $Q sends: C24.Name: Name of the assigned value C24.Value: Value C24.Unit: Unit of the assigned value C26.ActN: Number of single results C26.Mean: Mean (decimal places as for the result itself) C26.Std: Standard deviation (decimal places as for the result + 1) C26.RelStd: Relative standard deviation (in %, 2 decimal places) "RS1" "2.222" "%" "3" "3.421" "0.0231" "0.14" 3.2.2.66. Info.ActualInfo.Inputs.Status read only Info.ActualInfo.Inputs.Change read only Info.ActualInfo.Inputs.Clear $G Info.ActualInfo.Outputs.Status read only Info.ActualInfo.Outputs.Change read only Info.ActualInfo.Outputs.Clear $G Status sends the current status of the I/O lines, Change sends the information regarding whether a change in status of a line has taken place since the last clearing, Clear clears the change information. For the output, there is a conversion from binary to decimal, e.g. | 0 | 0 | 0 | 0 | 0 | 0 | 0 | 0 | 0 | 0 | 1 | 0 | 1 | 0 | Line No. | 13| 12| 11| 10| 9 | 8 | 7 | 6 | 5 | 4 | 3 | 2 | 1 | 0 | Output: 21 + 23 = "10" 1 means ON or change; 0 means OFF or no change. The lines are assigned as follows (see also page 125ff): Inputs: Outputs: 0 Start (pin 21) 0 Ready (pin 5) 1 Stop (pin 9) 1 Cond. ok (pin 18) 2 Enter (pin 22) 2 Titration (pin 4) 3 Clear (pin 10) 3 EOD (pin 17) 4 Smpl Ready (pin 23) 4 Monitoring, line L4 (pin 3) 5 pin 11 5 Error (pin 16) 6 pin 24 6 Activate, line L6 (pin 1) 7 pin 12 7 Pulse for recorder (pin 2) 8 not used (pin 6) 9 not used (pin 7) 10 not used (pin 8) 11 not used (pin 13) 12 not used (pin 19) 13 not used (pin 20) 3.2.2.67. Info.ActualInfo.Assembly.CyclNo read only $Q sends the current cycle number of the voltage measurement cycle, e.g. "127". From the cycle number and the cycle time (see 3.2.2.75), a time frame can be set up. The cycle number is set to 0 on switching on the instrument, on every start and for QuickMeas. It is incremented as long as the instrument remains switched on. 80 795 KFT Titrino 3.2 Remote control commands 3.2.2.68. Info.ActualInfo.Assembly.Counter.V read only Info.ActualInfo.Assembly.Counter.Clear $G $Q sends the volume. With the function &Info.Assembly.Counter.Clear $G, the volume counter is set to zero. 3.2.2.69. Info.ActualInfo.Assembly.Meas $Q sends the current measured value from the assembly. read only 3.2.2.70. read only read only read only read only read only read only read only Info.ActualInfo.Titrator.CyclNo Info.ActualInfo.Titrator.V Info.ActualInfo.Titrator.Meas Info.ActualInfo.Titrator.dVdt Info.ActualInfo.Titrator.dMeasdt Info.ActualInfo.Titrator.dMeasdV Info.ActualInfo.Titrator.T $Q sends the current values in the following formats: CyclNo V(mL) Meas: Ipol (mV) Upol (µA) dVdt (µL/s) dMeasdt Ipol (mV/s) Upol (µA/s) dMeasdV (mV/µL) KFT 127 1.2345 –345.6 –12.5 2.5142 0.7957 0.7957 10.6326 NV: Not Valid. OV will be sent for "overrange". A time frame can be set up from the cycle number and the cycle time (see 3.2.2.75). The cycle number is set to 0 at the start of a method and it is incremented until the end of the method. 3.2.2.71. Info.ActualInfo.MeasPt.Index read only Info.ActualInfo.MeasPt.X read only Info.ActualInfo.MeasPt.Y read only Info.ActualInfo.MeasPt.Z1 read only Info.ActualInfo.MeasPt.Z2 read only Info.ActualInfo.EP.Index read only Info.ActualInfo.EP.X read only Info.ActualInfo.EP.Y read only $Q sends the last entry into the measuring point list (.MeasPt) or the last entry into the list of EP's. 795 KFT Titrino 81 3.2 Remote control commands .MeasPt.X"165" Time of the MPList in s .MeasPt.Y"3.654" Volume of the MPList in mL .MeasPt.Z1"6.34" Measured value of the MPList, format depends on the measured quantity .MeasPt.Z2 without meaning .EP.X"1.234" Volume coordinate of the EP .EP.Y"5.34" Measured value coordinate of the EP 3.2.2.72. Info.ActualInfo.Oven.HeatTime read only Info.ActualInfo.Oven.SampleTemp read only Info.ActualInfo.Oven.LowTemp read only Info.ActualInfo.Oven.HighTemp read only Info.ActualInfo.Oven.GasFlow read only Info.ActualInfo.Oven.UnitFlow read only $Q sends the current values from a connected KF Oven. If no Oven is connected, the values are empty. .HeatTime: Heating time of sample in s. .SampleTemp: Nominal sample temperature in °C. .LowTemp: Lowest temperature during the sample heating time in °C. .HighTemp: Highest temperature during the sample heating time in °C. .GasFlow: Average gas flow during sample heating time. .UnitFlow: Unit of gas flow. 3.2.2.73. Info.ActualInfo.Display.L1 up to 32 ASCII characters Info.ActualInfo.Display.L8 up to 32 ASCII characters Info.ActualInfo.Display.DelAll $G Lines of the display. The display can be written to from the computer. Proceed as follows: 1. Lock the display, see 3.2.2.86. 2. Delete the whole display (.DelAll). 3. For writing onto the display, the standard character set will be used. 4. Unlock the display, see 3.2.2.86. 5. Delete the whole display (.DelAll). 6. Send a value to nod &Config.Aux.ResDisplay (see 3.2.2.46) to refresh the display. $Q sends the contents of the corresponding display line. 3.2.2.74. Info.ActualInfo.Comport.Number read only $Q sends the comport number of the Titrino where the PC is connected. 3.2.2.75. Info.Assembly.CycleTime read only Info.Assembly.ExV read only Inquiries regarding basic variables of the assembly: Cycle time in s, volume of the active Exchange Unit in mL. 82 795 KFT Titrino 3.2 Remote control commands 3.2.2.76. Assembly.Bur.Rates.Forward.Selected digital, analog Assembly.Bur.Rates.Forward.Digital 0...150, max. Assembly.Bur.Rates.Reverse.Selected digital, analog Assembly.Bur.Rates.Reverse.Digital 0...150, max. Expel and aspirating rate. Digital or analog control. With digital control, the inputted value applies (in mL/min). "max." means maximum possible rate with the Exchange Unit in current use. Analog means rate control with the analog potentiometer on Titrino. 3.2.2.77. Assembly.Bur.Fill $G starts the 'FILL' mode of the buret function. $G, $H, $C 3.2.2.78. Assembly.Bur.ModeDis $G, $S, $H, $C Assembly.Bur.ModeDis.Selected volume, time Assembly.Bur.ModeDis.V 0.0001...0.1...9999 Assembly.Bur.ModeDis.Time 0.25...1...86400 Assembly.Bur.ModeDis.VStop 0.0001...9999, OFF Assembly.Bur.ModeDis.AutoFill ON, OFF Dispensing mode with parameters. The dispensing mode can only be started and stopped via the RS Control. During a running dosification, no method can be started at the Titrino. .Selected: Dispensing of volume increments or during a preset time. .Volume, .Time: Size of the volume increments or entry of time. .VStop: Limit volume for the dispensing. .AutoFill: ON means automatic filling after every dispensing. 3.2.2.79. Assembly.Meas.Status Assembly.Meas.MeasInput Assembly.Meas.Ipol Assembly.Meas.Upol ON, OFF Ipol, Upol ±127...1...+127 ±1270...400...+1270 Measurement in assembly. The measuring function can only be started via RS Control. When the measuring function is switched on, no method can be started at the Titrino. .Input: Selection of the "measuring input" for polarized electrodes. .Ipol: Polarization current in µA. .Upol: Polarization potential in mV, entry in steps of 10 mV. 795 KFT Titrino 83 3.2 Remote control commands 3.2.2.80. Assembly.Outputs.AutoEOD ON, OFF Assembly.Outputs.SetLines $G Assembly.Outputs.SetLines.L0 active, inactive, pulse, OFF up to .L13 Assembly.Outputs.ResetLines $G Setting the I/O output lines. .AutoEOD: The automatic output of the EOD (End of Determination) at the end of the determination can be switched off. Thus, for example, in conjunction with a Titrino several determinations can be performed in the same beaker. Before AutoEOD is switched on, line 3 must be set to "OFF". .SetLines: With $G, all lines are set. .SetLines.LX: Set the line LX. "active" means setting of a static signal, "inactive" means resetting of the signal, "pulse" means output of a pulse of app. 150 ms, "OFF" means the line is not operated, see also page 126. Warnings: • If you have "AutoEOD" to "ON", an active line 3 is set to "inactive" by the EOD pulse. • L6 is the line of the activate pulse. An active line 6 is set to "inactive" by the activate pulse. • L5 is the error line. It is continuously controlled by the Titrino program and can therefore not be set freely. Line assignments in Titrino program: L0 Ready, inactive state L1 Conditioning OK L2 Titration in progress L3 EOD (End Of Determination) L4 --L5 Error L6 Activate pulse L7 Buret volume pulses L8–13 --.ResetLines: Lines are set to the inactive status (= high). 3.2.2.81. Assembly.Stirrer Switching stirrer ON/OFF. 3.2.2.82. Setup.Comport Selects the Titrino COM for the output of automatic info: &Setup.Keycode &Setup.Trace &Setup.SendMeas &Setup.AutoInfo 84 ON, OFF 1, 2, 1&2 795 KFT Titrino 3.2 Remote control commands 3.2.2.83. Setup.Keycode ON, OFF ON means the key code of a key pressed on the Titrino is outputted. The key code comprises 2 ASCII characters; table of the keys with their code, see page 102. A keystroke of key 11 is sent as follows: #11 The beginning of the message is marked by a space (ASCII 32). 3.2.2.84. Setup.Tree.Short ON, OFF Setup.Tree.ChangedOnly ON, OFF Definition of the type of answer to $Q. .Short: With "ON", each path is sent with only the necessary amount of characters in order to be unequivocal (printed in bold in this manual). A combination of .Short and .ChangedOnly is not possible. .ChangedOnly: Sends only the changed values, i.e. values which have been edited. All paths are sent absolute, i.e. from the root. 3.2.2.85. Setup.Trace ON, OFF The Titrino automatically reports when a value has been confirmed with <enter> at the Titrino. Message, e.g.: &SmplData.OFFSilo.Id1"Trace" The beginning of the message is marked by a space (ASCII 32). 3.2.2.86. Setup.Lock.Keyboard ON, OFF Setup.Lock.Config ON, OFF Setup.Lock.Parameter ON, OFF Setup.Lock.SmplData ON, OFF Setup.Lock.UserMeth.Recall ON, OFF Setup.Lock.UserMeth.Store ON, OFF Setup.Lock.UserMeth.Delete ON, OFF Setup.Lock.Display ON, OFF ON means disable the corresponding function: .Keyboard: Disable all keys of the Titrinos .Config: Disable the <configuration> key .Parameter: Disable the <parameter> key .SmplData: Disable the <smpl data> key .UserMeth.Recall: Disable "recall" in <user meth> key .UserMeth.Store: Disable "store" in <user meth> key .UserMeth.Delete: Disable "delete" in <user meth> key .Display: Disable the display, i.e. it will not be written to by the device program of the Titrino and can be operated from the computer. 795 KFT Titrino 85 3.2 Remote control commands 3.2.2.87. Setup.Mode.StartWait ON, OFF Setup.Mode.FinWait ON, OFF Holding points in the method sequence. If they are "ON", the sequence stops until "OFF" is sent. Switching the instrument on sets both nodes to OFF: .StartWait: Holding point right after starting a method (holding point after AutoInfo !".T.GC"). .FinWait: Holding point at the end a method (holding point after AutoInfo !".T.F"). 3.2.2.88. Setup.SendMeas.SendStatus ON, OFF Setup.SendMeas.Interval 0.08...4...16200, MPList .SendStatus: ON means the automatic transmission of measured values (see 3.2.2.90 and 3.2.2.91) in the inputted interval is active. .Interval: Time interval (in s) for the automatic transmission of associated measured values defined under points 3.2.2.90 and 3.2.2.91. The inputted value is rounded off to a multiple of 0.08. The smallest possible time interval depends on the number of measured values which have to be sent, on the baud rate, on the load on the interface and on the type of device connection. With "MPList" the measured values are sent at the time of their entry into the measured point list. The automatic transmission is switched on/off with 'SendStatus'. 3.2.2.89. Setup.SendMeas.Select Assembly, Titrator Selection of the unit of which the measured values should be sent (3.2.2.90 and 3.2.2.91). 3.2.2.90. Setup.SendMeas.Assembly.CyclNo ON, OFF Setup.SendMeas.Assembly.V ON, OFF Setup.SendMeas.Assembly.Meas ON, OFF Selection of the values from Assembly for the output in the set time interval (see 3.2.2.88): .CyclNo: Cycle number of the potential measurement. Together with the cycle time (3.2.2.75), a time frame can be set up. The cycle number is set to 0 on switching on the instrument and it is always incremented as long as the instrument remains switched on. .V: Volume .Meas: Measured value associated to the cycle number. The unit "assembly" must be preset (see 3.2.2.89). 3.2.2.91. Setup.SendMeas.Titrator.CyclNo ON, OFF Setup.SendMeas.Titrator.V ON, OFF Setup.SendMeas.Titrator.Meas ON, OFF Setup.SendMeas.Titrator.dVdt ON, OFF Setup.SendMeas.Titrator.dMeasdt ON, OFF Setup.SendMeas.Titrator.dMeasdV ON, OFF Selection of the values from the titrator which are sent in the set time interval (see 3.2.2.88, formats see 3.2.2.70): 86 795 KFT Titrino 3.2 Remote control commands .CyclNo: Cycle number. Together with the cycle time (see 3.2.2.75), a time frame can be set up. The other data belong to the corresponding cycle number. The cycle number is set to 0 at the start of a method and it is incremented until the end of the method. .V: Volume. .dVdt: associated volume drift. .dMeasdt: associated measured value drift. .dMeasdV: associated 1st derivative of the titration curve. The unit "titrator" must be preset (see 3.2.2.90). 3.2.2.92. Setup.AutoInfo.Status ON, OFF Setup.AutoInfo.P ON, OFF Setup.AutoInfo.T.R ON, OFF Setup.AutoInfo.T.G ON, OFF Setup.AutoInfo.T.GC ON, OFF Setup.AutoInfo.T.S ON, OFF Setup.AutoInfo.T.B ON, OFF Setup.AutoInfo.T.F ON, OFF Setup.AutoInfo.T.E ON, OFF Setup.AutoInfo.T.H ON, OFF Setup.AutoInfo.T.C ON, OFF Setup.AutoInfo.T.O ON, OFF Setup.AutoInfo.T.N ON, OFF Setup.AutoInfo.T.Re ON, OFF Setup.AutoInfo.T.Si ON, OFF Setup.AutoInfo.T.M ON, OFF Setup.AutoInfo.T.EP ON, OFF Setup.AutoInfo.T.RC ON, OFF Setup.AutoInfo.C.B1 ON, OFF Setup.AutoInfo.C.R1 ON, OFF Setup.AutoInfo.C.B2 ON, OFF Setup.AutoInfo.C.R2 ON, OFF Setup.AutoInfo.I ON, OFF Setup.AutoInfo.O ON, OFF ON means that the Titrino reports automatically the moment the corresponding change occurs. .Status: Global switch for all set AutoInfo. .P PowerOn: Simulation of power on (3.2.2.94). Not from mains. Messages from node .T, Titrator: .T.R Ready: Status 'Ready' has been reached. .T.G Go: Instrument has been started. .T.GC GoCommand: Instrument has received a go command. .T.S Stop: Status 'Stop' has been reached. .T.B Begin of sequence. .T.F Final: End of determination, the final steps will be carried out. .T.E Error. Message together with error number, see page 49ff. .T.H Hold: Status 'Hold' has been reached. .T.C Continue: Continue after hold. .T.O Conditioning OK: EP reached (in KFT with conditioning). .T.N Conditioning Not OK: EP not reached (in KFT with conditioning). .T.Re Request: In the inquiry of an identification or the sample size after start of titration. 795 KFT Titrino 87 3.2 Remote control commands .T.Si SiloEmpty: Silo empty, i.e. the last line has been removed from the silo memory. .T.M MeasList: Entry in the measuring point list. .T.EP EPList: Entry into EP list .T.RC Results have been recalculated. Messages from node .C, Comport: .C.B1 COM1: A report is outputted on COM1. During this time, COM2 will be blocked. COM2 is generally blocked, if COM1 is busy. .C.R1 COM1 is ready again. (Comes also when you <QUIT> an error.) .C.B2, .R2 Identical for COM2. Messages for changings in the I/O lines. If the changings are made simultaneously, there is 1 message. Pulses receive 2 messages: one message each for line active and inactive. .I Input: Change of an input line. .O Output: Change of an output line (except 7, pin 2, for recorder pulses). If a change occurs that requires a message, the Titrino sends space (ASCII 32) and ! as an introducer. This is followed by the name of the device (see 3.2.2.47). Special ASCII characters in the device name are ignored. If no device name has been entered, only ! is sent. Finally the Titrino sends the information which node has triggered the message. Example: !John".T.Si": The message was triggered from instrument "John", node .T.Si 3.2.2.93. Setup.Graphics.Grid ON, OFF Setup.Graphics.Frame ON, OFF Setup.Graphics.Scale Full, Auto Setup.Graphics.Recorder.Right 0.2...0.5...1.00 Setup.Graphics.Recorder.Feed 0.01...0.05...1.00 Change in the appearance and the format of the curve for the output. The settings are valid for both Titrino COM ports. .Grid: On/off switching of grid over curve. .Frame: On/off switching of frame surrounding the curve. If grid and frame are switched off, the curve is printed faster as the print head does not have to move to the end of the paper. .Scale: Type of scaling of the measured value axis: Full means that the scale runs from the smallest up to the greatest measured point. With auto, the smallest measured value is taken and the next smaller tick defines the beginning of the scale; the next greater tick to the greatest measured value is the end of the scale. .Right: Relative specification of the width of the output medium (e.g. paper width) for the length of the measured value axis. 1 means the measured value axis is plotted over the entire width of the paper (largest possible width). In extreme cases, the writing of the right tick may lie outside. 88 795 KFT Titrino 3.2 Remote control commands .Feed: Length of the time axis. Depending on the printer, the measure in cm may not always be correct. Curve length 0.01 100 cm 0.1 10 cm 0.5 2 cm 1 1 cm 3.2.2.94. Setup.PowerOn $G Simulation of 'power on'. The device has the same status as after power on: The cylinder is filled, error messages deleted and the current sample number set to 0. The method last used is ready for operation. 3.2.2.95. Setup.Initialise Setup.Initialise.Select $G ActMeth, Silo, Config, Assembly, Setup, All Setting of default values for the following areas: ActMeth: Current method. Parameters, calculations, and assignments for the data output, operands C01...C19. Silo: The silo memory is deleted. Same function as delete entire silo. Config: All values under &Config. Assembly: All values under &Assembly. Setup: All values under &Setup. All: Values of the entire tree (except silo and method memory). The action must be triggered with &Setup.Initalise $G. 3.2.2.96. Setup.RamInit $G Initializes instrument, see page 110. All parameters are set to their default value and error messages are cleared. The user and silo memories will be deleted. The user memory contains the default user methods from Metrohm. 3.2.2.97. Setup.InstrNo $G Setup.InstrNo.Value serial number, 8 ASCII characters Instrument identification for report output. Set the value with &Setup.InstrNo $G . 3.2.2.98. Diagnose.Report $G Output of the report containing the adjustment parameters. The Titrino has to be in its inactive basic state. 795 KFT Titrino 89 3.3 Properties of the RS 232 Interface 3.3 Properties of the RS 232 Interface Data Transfer Protocol The Titrino is configured as DTE (Data Terminal Equipment). The RS 232 interface has the following technical specifications: • Data interface according to the RS 232C standard, adjustable transfer parameters, see pages 11 and 75. • Max. line length: 512 characters • Control characters: CR (ASCII DEC 13) LF (ASCII DEC 10) XON (ASCII DEC 17) XOFF (ASCII DEC 19) • Cable length: max. approx. 15 m Start 7 or 8 Data Bit Parity Bit 1 or 2 Stop Bit Only a shielded data cable (for example, METROHM D.104.0201) may be used to couple the Titrino with foreign devices. The cable shield must be properly grounded on both instruments (pay attention to current loops; always ground in a star-head formation). Only plugs with sufficient shielding may be used (for example, METROHM K.210.0381 with K.210.9045). 3.3.1 Handshake Software-Handshake, SWchar Handshake inputs on the Titrino (CTS) are not checked. Handshake outputs (DTR, RTS) are set by the Titrino. The Titrino sends XOFF when its input buffer contains 384 characters. After this it can receive 128 extra characters (including LF). Titrino as Receiver : Titrino external device max. 128 characters RxD LF Data output 384 characters XOFF XON Data input TxD Time 90 795 KFT Titrino 3.3 Properties of the RS 232 Interface Titrino as Sender : Titrino external device XOFF XON Data output RxD LF Data input TxD max. characters max. characters: Data output disabled Data output enabled Time 2 characters at 300...9600 baud 16 characters at ≥ 19200 baud Software-Handshake, SWline Handshake input ports on the Titrino (CTS) are not checked. Handshake output ports (DTR, RTS) are set by the Titrino. The Titrino has an input buffer which can accept up to 512 characters. Titrino as Receiver : Titrino external device max. 128 characters RxD LF Data output 384 characters XOFF XON Data input TxD Time 795 KFT Titrino 91 3.3 Properties of the RS 232 Interface Titrino as Sender: Titrino external device XOFF XON Data output RxD 1st line LF 2nd line LF Data input TxD Data output disabled Data output enabled Time Titrino transmission can be stopped by external instruments with XOFF. After XOFF is received the Titrino completes sending the line already started. If data output is disabled for more than 6 s by XOFF, E43 appears in the display. Hardware-Handshake, HWs Titrino as Receiver : Titrino external device DTR RxD DTR LF RxD Time Titrino as Sender: Titrino external device RTS RTS CTS CTS TxD LF TxD Time The data flow can be interrupted by deactivating the CTS line. 92 795 KFT Titrino 3.3 Properties of the RS 232 Interface 3.3.2 Pin Assignment RS232C Interface Transmitted Data (TxD). If no data are transmitted, the line is held in the “ON” condition. Data will only be sent when CTS is in the ”ON” condition. Pin 3 Transmitted Data Pin 2 Received Data (RxD) Received Data Request to Send (RTS) ON condition: Titrino is ready to send data. Pin 7 Clear to Send (CTS) ON condition: Remote station is ready to receive data. Pin 8 Request To Send Clear To Send Pin 5 Signal ground (GND) Signal Ground Data Terminal Ready (DTR) ON condition: Instrument is ready to receive data. Pin 4 Data Terminal Ready Protective earthing Direct connection from cable plug to the protective ground of the instrument. Polarity allocation of the signals - Data lines (TxD, RxD) voltage negative (<–3 V): signal state ”ON” voltage positive (>+3 V): signal state ”ZERO” - control or message lines (CTS, RTS, DTR) voltage negative (<–3 V): OFF state voltage positive (>+3 V): ON state In the transitional range from +3 V to –3 V the signal state is undefined. Driver 14C88 according to EIA RS 232C specification Receiver 14C89 " " 795 KFT Titrino 93 3.3 Properties of the RS 232 Interface Contact arrangement at plug (female) for RS 232C socket (male) 6 9 1 5 View of soldered side of plug Ordering numbers: K.210.0381 and K.210.9045 No liability whatsoever will be accepted for damage or injury caused by improper interconnection of instruments. 94 795 KFT Titrino 3.3 Properties of the RS 232 Interface 3.3.3 What can you do if the data transfer does not work? Problem Questions for remedial action No characters can be received on a connected printer. - Are the instruments switched on and cables plugged in correctly? Is the printer set to ”on-line”? Are baud rate, data bit and parity the same on both instruments? - Is the handshake set properly? If everything seems to be ok, try to print a report with the key sequence <PRINT><SMPL DATA><ENTER>. If this report is printed out correctly, check if reports are defined in key <DEF>. No data transmission and the display of the Titrino shows an error message. - error 42: Transmission error. Is the printer set to "on-line"? Is the connection cable properly wired? error 43: Data output of the Titrino disabled for longer than 6 s by XOFF. error 36-39: Receive error. Are the RS settings the same on both devices? The received characters are garbled. - Wrong line spacing. The printer does not emulate completely the preset mode. Usually these problems arise with the IBM mode. Set the printer to a different mode (e.g. Epson). Printout of titration curve is not ok. Other reports are printed ok. Handshake is necessary for the printout of curves. - Is your cable correctly wired? (The DTR of the printer has to be connected to the CTS of the Titrino.) - Set "HWs" for the handshake of the Titrino. Configure the printer such that its DTR is set (possibly with DIP switches). 795 KFT Titrino Are the RS settings the same on both devices? Has the correct printer been selected? Data transfer has been interrupted on the hardware side during the printout of a curve. Re-establish connections and switch printer off/on. 95 4.1 Error and special messages 4 Error messages and Troubleshooting Data transfer inoperative See measures on page 95. 4.1 Error and special messages XXX bytes missing check electrode check exchange unit! check remote box division by zero error 36 error 37 error 38 error 39 error 42 error 43 795 KFT Titrino For the storage of a method or a silo line XXX bytes are missing. Remedy: <QUIT>. Delete methods no longer needed or use fewer silo lines. With polarized electrodes. There is a break or short circuit. Possible causes and rectification of the fault: - the electrode is not plugged in ⇒ plug it in - the electrode is not immersed in the solution ⇒ immerse it - the electrode is defective ⇒ use new electrode. - the electrode cable is defective ⇒ use new cable. The electrode test can be switched off under the <PARAM> key. Exit: Rectify fault or <STOP>. The Exchange Unit is not mounted (properly). Exit: Mount Exchange Unit (properly) so that the coupling engages or <STOP>. The Remote Box is not (correctly) connected or the Remote Box is connected but not activated under the <CONFIG> key. Exit: Connect Remote Box (correctly) and set "Remote Box: ON" under <CONFIG>, >peripheral units. Switch the Titrino off/on. The result could not be calculated as a divisor in the formula was equal to zero. Exit: Enter appropriate value. Parity Exit: <QUIT> and set corresponding quantity the same on both instruments Stop bit Exit: <QUIT> and set corresponding quantity the same on both instruments Overrun error. At least 1 character could not be read. Exit: <QUIT> Overflow of the receive buffer of the Titrino (> 128 characters). Exit: <QUIT> CTS=OFF Handshake unsatisfactory for more than 1 s. Exit: <QUIT> Is the receiver switched on and ready to receive? The transmission of the Titrino has been interrupted with XOFF for at least 6 s. Exit: <QUIT>. 97 4.1 Error and special messages error 45 manual stop meas.pt list overflow missing EP no new com.var. no new mean no new silo result no oven param. no titration data not valid overrange result out of limits sample size out service is due silo empty silo full 98 The receive buffer of the Titrino contains an incomplete string (missing LF). Transmission of the Titrino is thus blocked. Exit: Send LF or <QUIT>. The determination has been manually stopped. Maximum 500 measured points can be stored. Exit: Use start criteria or select larger time interval. An EP needed for calculation in a formula is missing. The common variable could not be assigned as the result or the mean value could not be calculated. The old value remains in force. No new mean value has been calculated as at least one quantity stipulated for mean value calculations could not be calculated. No new silo result C24 or C25 could be stored as the assigned quantity could not be calculated. The oven could not be found at the given COM. Remedy: connect the oven to the given RS-interface of the Titrino or set the following in your method under <PARAM>, >preselections, "Oven: no". No curve can be printed as no data are available. A value is not available. The measuring range of ±2 V has been exceeded. Overrange replaces the corresponding measured value (U or I). If a measured value is in overrange (primary or secondary measured value), the other (secondary or primary measured value) can also be unstable. The result lies outside the limits which were defined in the method, see page 26. Exit: Calculate result again or new start. The sample size is outside the limits which are defined in the method, see page 19. Exit: Enter new sample size. The service interval has elapsed. Contact Metrohm service so that the Titrino can be serviced. This message will appear each time the Titrino is switched on. Exit: New start. The silo memory is switched in but empty and a titration has been started. Corrective action: At least the first 1 silo line before starting the first titration. Exit: <CLEAR>. The silo memory is full up. Corrective action: If you have filled less than 255 silo lines, you can create more space by deleting old methods no longer needed. 1 silo line needs 18...120 bytes. Exit: <CLEAR>. 795 KFT Titrino 4.1 Error and special messages stop V reached system error 3 system error 14 time-out PC keyboard transmission error validate instrument wrong sample 795 KFT Titrino The determination has been stopped as the stop volume has been reached. The instrument adjustment data have been overwritten. Exit: <CLEAR>. Default adjustment data are set. The error message appears each time the instrument is switched on until it has been readjusted (Metrohm service). No communication between the Titrino and the connected Remote Box. Possible causes: . The Remote Box was connected when the Titrino was running . Titrino has a fault. . Remote Box has a fault. Remedy: Set under <CONFIG>, >peripheral units, "Remote Box: OFF", switch off Titrino, take away Remote Box and switch on Titrino. Contact Metrohm service. A connected PC keyboard has been used to call up an address (e.g. <F12>) and the connection has then been interrupted. Possible causes: . Remote Box has a fault. . PC keyboard has a fault. Exit: Correct fault and switch Titrino off/on. With a Remote Box connected characters are received which cannot be interpreted. Possible causes: . Wrong key combination has been pressed. . Wrong PC keyboard has been selected. . The barcode reader supplies garbled characters. . The Remote Box has a fault. Exit: Rectify fault and switch Titrino off/on. Validation interval has elapsed. Exit: <CLEAR> or new start. With KFT with preset titration direction, the first measured value is outside the end point. 99 4.2 Diagnosis 4.2 Diagnosis 4.2.1 General The 795 KFT Titrino is a very precise and reliable instrument. Thanks to its rugged construction it is virtually impossible for external mechanical or electrical influences to have an adverse effect on its functions. Although the occasional fault in the instrument can not be excluded completely, it is certainly much more likely that malfunctions are caused by wrong operation or handling or through improper connections and operation with non-Metrohm instruments. It is advisable in each case to isolate the fault with the rapid and easy to perform diagnostic tests. The customer thus need not call METROHM service until there is a true fault in the instrument. In addition, with the aid of the numbering in the diagnostic program he can provide the service engineer with much more accurate information. In inquiries always quote the manufacturing (page 5) and program number (see configuration, page 11) and specify possible error displays. 4.2.2 Procedure • The diagnostic steps must be performed in sequence and compared with the reactions of the 795 KFT Titrino (indented). In the "yes" case, continue with the next instruction. • If the instrument does not show the expected reaction ("no" case), the appropriate diagnostic step must be repeated to exclude an operating error. With repeated wrong reactions, however, there is a strong possibility that a malfunction exists. • The diagnostic steps allow re-entry into the test routine for repetition if the following display appears: diagnose press key 0...9 If the instrument is in a subprogram of the diagnostic routine: Press <CLEAR>. If need be, switch the power off then on again after a few seconds. At the same time press key <9> until the above display appears. • If <CLEAR> has been pressed during the display of 'diagnose press key 0...9', the instrument returns to the user program. • Error display: An error is shown in the display as follows: error XX error number • If a fault causes the buret drive to stick at the top or bottom end of the cylinder, see page 111, point 4.4. 100 795 KFT Titrino 4.2 Diagnosis 4.2.3 Equipment required: − voltage calibrator, e.g. 1.773.0010 Metrohm pH Simulator − highly insulated interconnection cable 6.2108.060 − resistor switch-box, class 0.1 % (or resistor 14.3 k, 0.1 %) − cable 3.496.5070 − exchange units, if possible with different cylinder volumes (or 3.496.0070 dummy exchange unit) − stop watch or watch with second hand − digital or analogue voltmeter (if need be, connect a calibrated recorder) − 2 connecting cables with 4 mm banana plugs − test plug 3.496.8550 (necessary only if plug ‘Remote’ should be checked) − test plug 3.496.8560 (necessary only if plug ‘RS 232’ should be checked) or 1.767.0010 Calibrated Reference for mV, pH, Ω µS, °C 4.2.4 Diagnosis steps 1 Prepare instruments for diagnostic test • Power off. • Disconnect all external connections (cables at rear, except mains cable and keyboard). • Remove exchange unit. • Power on and immediately press and hold the <9> key until the powerup test pattern disappears. diagnose press key 0...9 2 Perform display test • Press <2>. display test • Press <ENTER>. Characters for a visual check of the display are generated on the eight lines. Test sequence: a) The display is cleared and overwritten from the top left to the bottom right with a dot pattern ( ▓▓▓▓▓▓▓▓ ). b) The display is cleared and overwritten from the top left to the bottom right with a dot pattern( ░░░░░░░░ ). c) The display is continuously cleared and overwritten from the top left to the bottom right with the complete character set. At the same time with moving display the LED’s „COND.“, „STATISTICS“ and „SILO“ are switches on and off. • The test sequence can be held and then continued at any time by pressing <5>. • Block 2 is quit by pressing <CLEAR>. diagnose press key 0...9 795 KFT Titrino 101 4.2 Diagnosis Fig. 1 Complete character set 3 Keypad test • Press <1>. keys test • Press <ENTER>. keys test matrix code • If any key is now pressed (on the 6.2130.070 keypad or on the front panel of the 795), the appropriate matrix code appears in the display. Fig. 3 Fig. 2 Front panel 795 Keypad 795 • Block 1 is quit by pressing the <CLEAR> key twice. diagnose press key 0...9 102 795 KFT Titrino 4.2 Diagnosis 4 Cylinder code, date, time • Insert exchange unit or dummy to the internal dosing unit D0 and put the buret tip into a collecting receptacle. • Press <0>. date/time cylinder code • Press <ENTER>. date YYYY-MM-DD code:D0 XX ml activated dosing unit hh:mm:ss mL-code • Check date and time. • Press <CLEAR>. diagnose press key 0...9 5 Motor timer test • Press <6>. motor-timer test • Press <ENTER>. pot.meter dV/dt 10? • Turn knob 'dV/dt' to the right stop and press <ENTER>. Test sequence: a) In a first step, the frequency of the RC oscillator (analogue rate) is tested over a period of 1 second. b) In a second step, the frequency of the quartz oscillator (digital rate) is tested over a period of 1 second. c) If no error is found, after about 5 s it appears motor-timer test o.k. • Press <CLEAR>. diagnose press key 0...9 795 KFT Titrino 103 4.2 Diagnosis 6 Measuring input test: Polarizer test With the aid of the "767.0010 calibrated reference for mV, pH, Ω, µS, °C" you can check the measuring input "Pol". If a Remote Box is connected: Deactivate the Remote Box (key <Config>, >peripheral units, Remote Box: off"). Switch the Titrino off and screw off the Remote Box. Switch the Titrino on again (so that the new configuration will be recognized). • Press <7>. polarizer test • Press <ENTER>. dummy resistor 14.3 kΩ • Screw off electrode cable (6.2104.020) and insert in socket 5 of the 767 (the cover remains closed on the 767) or connect resistor switch box (14.3 kΩ) using 3.496.5070 cable to ‘Pol’ socket. • Press <ENTER>. Test sequence: 1. An asterisk flashes during the test. 2. In case of an error an error message appears. (If for example the switch-box is not connected, error 100 appears). 3. If no error is found, after about 15 s display shows polarizer test o.k. • Press <CLEAR>. diagnose press key 0...9 • Remove 767 or cable and resistor switch-box. 104 795 KFT Titrino 4.2 Diagnosis 7 External inputs and outputs This test is meaningful only if the 795 KFT Titrino is used interconnected with other instruments via the 'Remote' connection or if the 6.2148.000 remote box is used for connecting a PC keyboard or a barcode reader.If the remote box should be tested, it has to be connected to the Titrino before the Titrino is switched on. In addition, a 3.496.8550 test plug normally used in the repair service is required for this test. However, this plug can also be purchased by customers under the above number. For the sake of completeness, the procedure is described here. If a diagnostic test of the external inputs and outputs is not required, continue with point 8. 5 Fig. 4 18 4 17 3 16 1 2 6 7 8 13 19 20 12 24 11 23 10 22 9 21 Connections in the 3.496.8550 test plug • Press <4>. extern i/o test 1...2 7.1 Test of the remote interface • Press <1>. extern input/output test • Press <ENTER>. I/O-test-connector? • Insert the 3.496.8550 test plug in port B 'Remote'. (Do not switch off instrument!) • Press <ENTER>. Test sequence: 1. In case of an error an error message is displayed. If for example no test plug is connected, error message error 50 01HEX appears). 2. If no error is found, after about 1 s display shows extern input/output o.k. • Remove test plug. • Press <CLEAR>. extern i/o test 795 KFT Titrino 1...2 105 4.2 Diagnosis 7.2 Test of the remote box The remote box needs to be connected before the Titrino is switched on. Insert 3.496.8550 test plug in the remote box. • Press <2>. reset remote box? • Press <ENTER>. Test sequence: 1. In case of an error an error message is displayed (for example error 490 01HEX). 2. If no error is found, after about 1 s display shows remote box test o.k. • Press <CLEAR>. The dialogue switches automatically to the "extern i/o test". extern input/output test • If this test should not be carried out (see 7.1), quit block 4 pressing <CLEAR> twice. • Remove test plug. diagnose press key 0...9 8 RS 232 test A 3.496.8560 test plug normally used in the repair service is required for this test. However, this plug can also be purchased by customers under the above number. For the sake of completeness, the procedure is described here. If a diagnostic test of the RS 232 interface is not required, continue with point 9. 2 Fig. 5 3 8 20 6 4 5 Connections in the 3.496.8560 plug • Press <5>. RS232 test 106 1...2 795 KFT Titrino 4.2 Diagnosis 8.1 RS232 test 1 • Press <1>. RS232 test-connector? 1 • Insert the 3.496.8560 test plug in port ‘A1’. • Press <ENTER>. Test sequence: 1. In case of an error an error message is displayed. If for example no test plug is connected, error message error 69 appears). 2. If no error is found, after about 5 s display shows RS232 test 1 o.k. • Remove test plug. • Press <CLEAR>. RS232 test 1...2 8.2 RS232 test 2 • Press <2>. RS232 test-connector? 2 • Insert the 3.496.8560 test plug in port ‘A2’. • Press <ENTER>. Test sequence: 1. In case of an error an error message is displayed. If for example no test plug is connected, error message error 69 appears) 2. If no error is found, after about 5 s display shows RS232 test 2 o.k. • Remove test plug. • Press <CLEAR>. RS232 test 1...2 • Press <CLEAR>. diagnose press key 0...9 795 KFT Titrino 107 4.2 Diagnosis 9 Internal dosing unit • Remove exchange unit. • Check spindle zero position, see Fig. 5. 0.2 - 0.6 mm Fig. 6 Fig. 7 The spindle must be 0.2 – 0.6 mm below the edge of the sliding plate. The bar of the stopcock coupling must be exactly parallel to the lateral edges of the KFT Titrino, see Fig.6. • Reinsert Exchange Unit. Titrino fills. The display of before reappears. • Knob 'dV/dt' to right stop. • Press the <DOS> key (on instrument) until the piston rod reaches the top and at the same time measure the time from start to end. XXX X ******** cylinder empty ! mind selected language! Spindle remains at maximum position. The transit time of the spindle is 20 s. • Measure spindle lifting (can be performed only if the 3.496.0070 Dummy Exchange Unit is inserted or the locking switch (in right hole) is carefully operated with a screwdriver after removal of the Exchange Unit). From the start point, the spindle travels 80 mm. Instead of the spindle height, the expelled volume can be measured (corresponds to max. vol. of Exchange Unit used). • Press <FILL> (on instrument) and simultaneously measure the time until the KFT Titrino is again in the 'ready' position. Times for filling: per stop cock cycle for filling 1s 20 s (Tolerance: 10 %) The following generally holds: Spindle and stopcock must move at a constant speed (noise!). In the filling setting, the stopcock coupling must position the lever of the Exchange Unit correctly at the left stop (with virtually no play and without sticking). • Set potentiometer 'dV/dt' to left stop. • Press <DOS> (on instrument) at same time and use a stopwatch to measure the time for 1/10 of the cylinder volume to be expelled. The time should be ca. 90...110 s. • Set potentiometer 'dV/dt' to right stop. • Press <FILL>. 108 795 KFT Titrino 4.2 Diagnosis 10 Setting up original arrangement Reconnect all peripherals disconnected at the start of the diagnostic routine and perform a short function test with these. 795 KFT Titrino 109 4.3 Initialize and test RAM 4.3 Initialize and test RAM On the odd occasion large disturbing signals (e.g. mains spikes, lightning, etc.) can have an adverse effect on the processor functions and hence lead to a system crash. After such a crash the RAM area must be initialized. Although the basic instrument data remain stored, the RAM initialization should be performed only when necessary since the stored user data (configuration, parameters, calculation variables, etc.) are cleared as a result. • Power OFF • Power ON and simultaneously press keys <DOS> and <STOP/FILL>. RAM Init. • Press <START>. confirm RAM Init. • Press <START>. RAM Init. activ RAM is tested and initialized. Subsequently a warm start is executed. The lost data of the user memory must now be reentered. If 'system error 3' appears in the display, <CLEAR> can be used to return to the instrument program. The initialization values are loaded automatically. The instrument thus remains capable of measurement. However, possibly a small loss in accuracy must be anticipated. A new optimum adjustment can be performed by Metrohm service. The error message 'system error 3' always appears after the instrument is switched on until this adjustment has been performed. 110 795 KFT Titrino 4.4 Releasing a locked spindle 4.4 Releasing a locked spindle with inserted Exchange Unit • The buret drive may very occasionally jam at the top or bottom end of the cylinder. If jamming occurs at the top or when the drive is out of function, the Exchange Unit can no longer be removed. In this case, it is necessary to proceed as follows: 2 screws (M4 countersunk) 2 screws (M3 fillister head) knob edge of bench Fig. 8 • Disconnect instrument from power supply! • Remove control knob. • Place instrument over edge of bench to allow the M3 screws to be removed (Fig. 7). • Remove M4 screws. • Lift off top part of instrument together with Exchange Unit in the manner shown by the arrow. The electronic circuits are now accessible! On no account touch these! • Remove spindle from mechanical stop by turning the large gear wheel. (In case that the motor is inoperative, position spindle by hand to zero position.) 795 KFT Titrino 111 5.1 Setting up and connecting the instruments 5 Preparations The mains cables supplied with the instrument are three-core and equipped with a plug with an earthing pin. If a different plug has to be fitted, the yellow/green lead must be connected to the protective earth. Each break in the earthing inside or outside the instrument can make it a hazard. When the instrument is opened or if parts of it are removed, certain components may be live if the instrument is connected to the mains. The mains cable must therefore always be unplugged when certain adjustments are made or parts replaced. When peripheral instruments are connected to the KFT Titrino, the Titrino and the instruments to be connected have to be switched off, otherwise all instruments could suffer damage! Before connecting a printer or a balance to the RS232 Interface, switch off the Titrino! 5.1 Setting up and connecting the instruments 5.1.1 Titrino with Stirrer or Titration Stand A C B 795 D Stirrer cable Stirrer or Ti Stand 6.2130.070 Keypad The 802 Rod Stirrer, the 727, or the 703 Ti Stand with 6.2108.100 cable can also be connected instead of the 728 Magnetic Stirrer. 112 795 KFT Titrino 5.1 Setting up and connecting the instruments 5.1.2 Connection of a printer A variety of printers can be connected to the RS232 interface of the Titrino. If you connect a printer other than one of those mentioned below, ensure that the Epson mode is emulated or that it uses the international character set following the IBM Standard Table 437 and IBM-compatible graphics control characters. If a balance is connected at the same COM of the Titrino as a printer, you need the 6.2125.010 + 6.2125.030 Adapters. Printer Seiko DPU-414 Cable 6.2134.110 Custom DP40-S4N 6.2134.110 Citizen iDP562 RS 6.2134.050 Epson 6.2134.050 LX-300+ HP Desk Jet 6.2134.050 with serial interface HP Desk Jet 2.145.0330 with parallel RS232/ interface Parallel Converter 795 KFT Titrino Settings on Titrino baud rate: 9600 data bit: 8 stop bit: 1 parity: none handshake: HWs send to: Seiko baud rate: 9600 data bit: 8 stop bit: 1 parity: none handshake: HWs send to: Citizen baud rate: data bit: stop bit: parity: handshake: send to: as above, but send to: baud rate: data bit: stop bit: parity: handshake: send to: baud rate: data bit: stop bit: parity: handshake: send to: 9600 8 1 none HWs Citizen Epson 9600 8 1 none HWs HP 9600 8 1 none HWs HP Settings on Printer none none, pre-set on Metrohm version IDP-560 EMULATION FONT MAP =GERMANY PRINT=REVERSE LITTLE CR CODE=VOID CR AFTER B :FULL=VOID CR ON b. EMPTY=VALID BUFFER 1K BYTE BAUD RATE=9600 PROTOCOL=8,N,1 FLOW CONTROL CTS-RTS ON 1 2 3 4 5 6 7 8 9 10 SSW1 see printer manual A: A4 Paper 1 2 3 4 5 6 7 8 1 2 3 4 5 6 7 8 B: see printer manual 113 5.1 Setting up and connecting the instruments 5.1.3 Connection of a balance The following balances can be connected to the RS232 output of the Titrino: Balance Cable Sartorius MP8, MC1 6.2134.060 Shimadzu BX, BW 6.2125.080+6.2125.010 Settings on Ohaus Voyager, Explorer, Analytical Plus Titrino: Balance: balance delimiter SARTORIUS CR+LF from Ohaus: AS017-09 (Ohaus parts number) Settings on Titrino: Balance: balance SARTORIUS SET BALANCE INTERFACE BAUD RATE DATA BITS PARITY STOP BITS 9600 8 none 1 Mettler AB, AG (LC-RS25) in the scope of delivery of the balance Mettler AM, PM 6.2146.020 + 6.2125.010 additionally from Mettler: ME 47473 Adapter and ME 42500 hand switch or ME 46278 foot switch Mettler interface 016 Cable in scope of delivery of interface 016: Red lead to pin 3, white lead to pin 7 of the 25-pin connector + 6.2125.010 25 Pol/9 Pol Adapter Mettler interface 011 or 012 6.2125.020 + 6.2125.010 Mettler AT 6.2146.020 + 6.2125.010 Mettler PG, AB-S 6.2134.110 Mettler AX,MX, UMX 6.2134.120 AND Models ER-60, 120, 180, 182 6.2125.020 + 6.2125.010 Models FR-200, 300 Models FX-200, 300, 320 with RS232 interface (OP-03) Precisa, balances with RS232Cinterface 6.2125.080 + 6.2125.010 The balance type must be preselected at the Titrino with the <CONFIG> key. The weight is transferred as a number with up to 6 digits, sign and decimal point. Units and control characters sent by the balance are not transmitted. With the aid of a special input unit supplied by the balance manufacturer, in addition to the weight identifications and methods can be 114 795 KFT Titrino 5.1 Setting up and connecting the instruments inputted from the balance. For this, the address of the identifications and method, resp. must be preselected on the input unit. Balance Sartorius Mettler (AT) Method METH or 27 D (Mthd) Id1 ID.1 or 26 C (ID#1) Id2 ID.2 or 24 B (ID#2) Id3 C-20 or 23 A (c20) If balance and printer are connected at the same Titrino COM you need the 6.2125.010 and 6.2125.030 Adapters. If the balance works only with 7 bit and the printer with 8 bit and if they are at the same Titrino COM, the balance has to bet to "space parity" and Titrino/printer to 8 bit, "no parity". 5.1.4 Connection of a KF Oven It is expedient to place the oven on 6.2041.180 instrument bridge. Take care that the gas outlet of the oven enters the titration vessel as directly as is possible to prevent the formation of condensed water in the outlet tubing. Oven on 6.2041.180 instrument bridge Connection of both RS interfaces (cable 6.2125.110) is only necessary when you require the oven results in the 795 Titrino report. Make sure there is no report output from the oven! A C B 795 768 D A B C D 6.2141.010 Cable (Remo6.2125.110 Cable (RS) 795 KFT Titrino 115 5.1 Setting up and connecting the instruments When the RS interfaces are not connected then the following setting must be made at the Titrino: <PARAM>, >preselections, "Oven: no". If you enter one of the COMs of the Titrino for this parameter then your Titrino result report will contain the oven data "heating time", "sample temp.", "lowest temp.", "highest temp." and "gas flow". The start is triggered at the oven. When the Titrtrino titration vessel has been conditioned the oven automatically starts the titration. The 707 KF Oven can also be connected instead of the 768 KF Oven. 5.1.5 Connection of a Sample Changer A C B 795 D 730 6.2141.020 Cable With 6.2141.030 cable (instead of 6.2141.020), two Titrinos can be connected to the 730 (or 760) Sample Changer at the same time. • The "Remote" socket allows not only connection of a sample changer but also additional control functions. Pin assignment of the "Remote" socket and control possibilities, see page 125. • If a calibration has to be performed with the sample changer, the calibration parameter "sample changer:" must be set to "ON". • In connections with the sample changer, "auto start" should be set to "OFF" in the <CONFIG> key. The start command is given by the Sample Changer. 116 795 KFT Titrino 5.1 Setting up and connecting the instruments 5.1.6 Connection of the 774 Oven Sample Processor The Oven Sample Processor heats the sample and transfers the moisture from the sample to the titration vessel of the Titino. Titrino and Oven Sample Processor are connected via the remote sockets (cable 6.2141.020) as well as via the RS interfaces (cable 6.2125.110) A C B 795 D 774 6.2141.020 Cable (Remote) 6.2125.110 Cable (RS 232) • The "Remote" socket allows not only connection of a sample changer but also additional control functions. Pin assignment of the "Remote" socket and control possibilities, see page 125. • In connections with the oven sample processor, "auto start" should be set to "OFF" in the <CONFIG> key. The start command is given by the oven sample processor. In addition, while a sequence is being processed, the 774 Oven Sample Processor can, via the serial RS interface, cause the 795 Titrino to load a particular method. The Titrino can obtain the oven parameters via the RS connection. 795 KFT Titrino 117 5.1 Setting up and connecting the instruments 5.1.7 Connection of a computer A C B 795 D 6.2134.040 Cable (9/9 pins) or 6.2125.010+6.2125.060 Cables (9/25 pins) PC Preselections on the Titrino: RS232 settings: ......................................... depend on the control program of the computer Send to:............................................................................................................................ IBM Vesuv 3.0, PC program for data acquisition and method backup for up to 64 devices ...................................................................................... 6.6008.200 for 2 devices.................................................................................................. 6.6008.500 5.1.8 Connection of a Remote Box A barcode reader and/or a PC keyboard can be connected to 6.2148.000 Remote Box. The barcode reader and PC keyboard are used as input aids. Only plug in and unplug the Remote Box when the Titrino is switched off! The Remote Box is screwed onto the "Remote" socket of the Titrino. The remote lines of the Titrino are then accessible at the "Remote" socket of the Remote Box. 5.1.8.1 Connecting a barcode reader Barcode readers with a 5-pole DIN plug can be connected to 6.2148.000 Remote Box. A precondition is that the barcode reader can emulate a PC keyboard. If a barcode reader and a PC keyboard are to be connected at the same time then the barcode reader must have a T-connection plug. The PC keyboard will then be plugged into this barcode reader connection. 118 795 KFT Titrino 5.1 Setting up and connecting the instruments Settings at the Titrino: Under key <CONFIG>, >peripheral units, "Remote Box: on" Barcode: input method id1 id2, id3 smpl size The barcode string goes to the entry field in which the cursor is currently located. If the silo memory is switched on the barcode string always goes to the method. The cursor position has no effect. If the silo memory is switched off the input has no meaning. The barcode string always goes to Id1. The cursor position has no effect. As for id1. The barcode string always goes to the sample size. The cursor position has no effect. If the silo memory is switched on the silo line will be concluded with the sample size and the cursor moves to the next silo line. Settings at the barcode reader: Plug the barcode reader into the Remote Box. The barcode reader instruction manual contains the codes which you must enter. 1. Bring the barcode reader into the programming mode. 2. Make the necessary setting for emulating a PC keyboard (may be country-specific). Select <ENTER> or "CR + LF" as termination sign. 3. Exit the programming mode. Notes: • If longer characters chains than are permitted by the corresponding input are transmitted then the first n characters will be accepted; the last characters will be cut off. • If the silo memory is switched on and the settings "barcode: method" or "barcode: idX" are operative, the first silo line will be created when the string is received. Higher silo lines than 1 are only created and concluded with the sample size. 5.1.8.2 Connecting a PC keyboard PC keyboards with a 5-pole DIN plug can be connected to 6.2148.000 Remote Box. For keyboards with a PS/2 plug an adapter PS/2→DIN is available in PC shops. Settings at the Titrino: Under key <CONFIG>, >peripheral units, "Remote Box: on" Keyboard: Select the country-specific keyboard layout of your PC keyboard. If the Titrino does not support your keyboard you should select a keyboard which has the closest possible layout (for example check the 2nd occupancy of the numerical keys). Country-specific special characters will probably not be converted correctly. 795 KFT Titrino 119 5.1 Setting up and connecting the instruments 5.1.8.3 Operating via a PC keyboard: The Titrino can be operated from the PC keyboard. The Titrino functions are called up as follows: Titrino function <C-FMLA> <CLEAR> <CONFIG> Cursor ↑ ↓ 120 Key combination on PC keyboard Alt F F5 F10 Cursor ↑ ↓ Cursor → ← Cursor → ← <DEF> DEF: formula input, common variable, mean value: EP RS MN C <ENTER> <MEAS/HOLD> <MODE> <PARAM> <PRINT> <QUIT> <REPORTS> Alt D E R M C enter F9 F2 F11 Alt P ESC Alt O <SILO> <SMPL DATA> <START> <STATISTICS> <STOP> <USER METH> <USER> F4 F12 F7 F6 F8 F3 Alt U Remarks Navigation, move the cursor along the curve Selection of inputs Change between result display and display of the curve (<CURVE>) Input of corresponding quantity or variable together with the numerical address, e.g. R1 gives RS1. Report selection with → ← Printout reports: Alt P + Alt O on/off on/off 795 KFT Titrino 5.1 Setting up and connecting the instruments The numerical block (with NumLock) and the number keys on the PC keyboard simulate the functions of the numerical keys on the Titrino. For example, entering <7> in the basic state of the Titrino switches the statistics on. Keys which are used for setting an accent (e.g. ^, ´) are converted immediately. If you try to enter ê the Titrino will display ^e instead. The occupancy of the PC function keys is shown to the right as an overlay. You can copy this diagram, cut out the central part and place it above the function keys of your PC keyboard. 795 Mode User Meth Silo Clear Statistics Start Stop Meas/Hold Config Param SmplData 795 KFT Titrino 121 5.2 Connection of electrodes and preparing titration vessel 5.2 Connection of electrodes and preparing titration vessel The Titrino 795 has one measuring input. Rear panel: Pol Pol Connection of polarized electrodes. If measured quantities Ipol or Upol are selected, this measuring input is automatically active. Setting up the KF titration vessel For volumetric KF titrations install the titration vessec according to the following figure: Electrode cable 6.2104.020 Double Pt-electrode 6.0338.100 Drying tube 6.1403.040 Screw nipple 6.2730.010 Stopper 6.2730.030 Stopper with septum 18 mm 6.2730.020 Titration vessel lid 6.1414.030 Septum 6.1448.010 Set of O-rings 6.1244.040 Magnetic stirring bar 6.1903.020 122 Titration vessel 20...90 mL 6.1415.220 795 KFT Titrino 6.1 Technical specifications 6 Appendix 6.1 Technical specifications Modes KFT: Karl Fisher Titration for water determination Measuring inputs 1 measuring input for polarized electrodes. Measuring range Voltage Current Water content 0...±2000 mV, resolution 1 mV, error limit 0.1 % full scale 0...±200.0 µA, resolution 1 µA a few ppm to 100 % Polarizer Ipol: 0...±127 µA, resolution 1 µA Upol: 0...±1270 mV, in steps of 10 mV Dosification Volume of buret cylinder Resolution Titrating burets Auxiliary burets 1, 5, 10, 20 or 50 mL 10 000 steps per buret cylinder 1 internal buret 1 additional buret: 765 or 776 Dosimat Materials Housing Keypad cover Polybutyleneterephthalate (PBTP) Polycarbonate (PC) Display Graphical LCD, 192 x 64 Dots Field: 100 x 37 mm LED back-lit Memory Method memory for up to 100 methods Data bank with 18 Metrohm methods Silo memory for sample data and results RS232 interface 2 separate interfaces, each can be configured for printer, balance or computer connection: completely controllable from external control unit Remote input/output lines 795 KFT Titrino for Sample Changer, robot connection, oven, ultra turax... With optional Remote Box: Connection of barcode reader and PC keyboard. 123 6.1 Technical specifications Stirrer control Ambient temperature Nom. operation range Storage Transport Safety specifications Mains connection Voltage Frequency Power consumption Fuse Switch the stirrer on/off either manually or coordinated with the titration sequence 5...40 °C –20...60 °C –40...60 °C Designed and tested in accordance to IEC publication 1010, safety class I. This manual contains information and warnings which have to be followed by the user to ensure safe operation and to retain the apparatus in safe condition. 100...240 V 50...60 Hz 15 W 2 x 1 ATH (to be replaced by Metrohm Service only using the same type) Additional electronic overload protection Dimensions with Exchange Unit Width 150 mm Height 450 mm Depth 275 mm Weight, incl. keypad 124 app. 3.6 kg 795 KFT Titrino 6.2 Pin assignment of the "Remote" socket 6.2 Pin assignment of the "Remote" socket external Inputs Function +5 V pin 21 (Input 0) Start pin 9 (Input 1) Stop +5 V +5 V tp pin 22 (Input 2) Enter pin 10 (Input 3) Clear tp > 100 ms Functions see page 127. +5 V Not used in titration sequences +5 V pin 23 (Input 4) +5 V Sample ready pin 11 (Input 5) +5 V pin 24 (Input 6) not used +5 V pin 12 (Input 7) Outputs 795 KFT Titrino pin 5 (Output 0) Ready inactive pin 18 (Output 1) Conditioning ok, active if Cond.ok pin 4 (Output 2) Titration, active during titration 125 6.2 Pin assignment of the "Remote" socket Outputs pin 17 (Output 3) End of determination EOD pin 3 (Output 4) not used pin 16 (Output 5) Error, active with errors pin 1 (Output 6) Activate pulse, see page 127. L6 in TIP pin 2 (Output 7) Pulses for recorder (tp=150 µs) 10 000 per buret cylinder pin 6 (Output 8) not used pin 7 (Output 9) not used pin 8 (Output 10) not used pin 13 (Output 11) not used pin 19 (Output 12) sample size out of limits pin 20 (Output 13) result out of limits, see page 26 For all outputs: VCE0 = 40 V = 20 mA IC tPulse > 100 ms Functions see page 127. Voltage +5 V pin 15 I ≤ 200 mA 0V pin 14 0 V: active 5 V: inactive pin 25 Ordering numbers for plug: K.210.9004 (shell) and K.210.002 No liability whatsoever will be accepted for damage caused by improper interconnection of instruments. 126 795 KFT Titrino 6.2 Pin assignment of the "Remote" socket 6.2.1 Lines of the "Remote" socket during the titration 795 KFT Titrino 127 6.2 Pin assignment of the "Remote" socket 6.2.2 Possible configurations of the activate pulse KFT first cond. all inactive START Conditioning START Request id... Start titration End of det. (EOD) Data output 128 795 KFT Titrino 6.3 User methods 6.3 User methods 6.3.1 General The methods are stored in the user memory ready for use. They can be loaded, modified and overwritten. Connect the printer to COM1 of the Titrino. If you have no printer connected, you have to delete the reports under the key <DEF>, >report. If the result should have another unit, you need to adjust the calculation constants using the key <C-FMLA>. The following methods are available: 'um 795 KFT Titrino 01103 user pkl date 2001-11-15 time user methods 795.0010 17:50 bytes – KF-titer with H2O or methanol standard KFT Ipol H2OTiter 152 – KF-titer with sodium tartrate KFT Ipol TarTiter 152 – Blank determination for KFT KFT Ipol Blank_KF 134 – KF-titration with blank value subtraction KFT Ipol KF-Blank 208 – KF-titration without blank value subtraction KFT Ipol KF 172 – KF-titer KFT Ipol 5Titer 152 – KF-titration without blank value subtraction KFT Ipol 5Deter 172 – KF-titration with blank value subtraction KFT Ipol 5Deter-B 208 – KF-titer KFT Ipol 2Titer 152 – KF-titration without blank value subtraction KFT Ipol 2Deter 172 – KF-titration with blank value subtraction KFT Ipol 2Deter-B 208 – KF-titer KFT Ipol 1Titer 152 – KF-titration without blank value subtraction KFT Ipol 1Deter 172 – KF-titration with blank value subtraction KFT Ipol 1Deter-B 208 – KF-titer KFT Ipol KetTiter 152 – KF-titration without blank value subtraction KFT Ipol KetDeter 172 – KF-titration with blank value subtraction KFT Ipol KetDet-B 208 – Bromine number according ASTM D 1159-84 KFT Ipol BrNumber 212 remaining bytes 96716 for KF reagent 5 mg/mL H2O for KF reagent 2 mg/mL H2O for KF reagent 1 mg/mL H2O for special ketone/aldehyde KF reagent ------------ 795 KFT Titrino 129 6.3 User methods 6.3.2 KF Titer determination with H2O or methanol standard "H2OTiter" 'pa 795 KFT Titrino 795.0010 date 2001-11-15 time 17:58 0 KFT Ipol H2OTiter parameters >control parameters EP at U 250 mV dynamics 100 mV max.rate max. ml/min min.volume incr. min. µl stop crit: drift stop drift 20 µl/min >titration parameters titr.direction: pause 1 0 s start V: OFF pause 2 0 s extr.time 0 s I(pol) 50 µA electrode test: OFF temperature 25.0 °C time interval 2 s >stop conditions stop V: abs. stop V 99.99 ml filling rate max. ml/min >statistics status: ON mean n= 5 res.tab: original >preselections conditioning: ON display drift: ON drift corr: OFF req.ident: OFF req.smpl size: value limit smpl size: OFF oven: no activate pulse: OFF -----------'fm 795 KFT Titrino 795.0010 date 2001-11-15 time 17:59 0 KFT Ipol H2OTiter >calculations Titer=C00/EP1*C01;4;mg/ml C00= 1.0 C01= 1000 ------------ 130 'de 795 KFT Titrino 795.0010 date 2001-11-15 time 17:59 KFT Ipol H2OTiter def >formula Titer=C00/EP1*C01 RS1 text Titer RS1 decimal places 4 RS1 unit: mg/ml RS1 limit control: OFF >silo calculations match id: OFF >common variables C39=MN1 >report report COM1:full; >mean MN1=RS1 >temporary variables ------------ The titer is calculated as mean value of 5 single determinations and stored as common variable C39. Therefore, it can be directly used in subsequent methods. Electrode: Double Pt-electrode 6.0338.100 at measuring input "Pol". Titrating agent: One-component or two-component KarlFischer reagent, ready to use. Solvent: 20 mL Methanol or a specific solvent, conditioned. Sample: Distilled water, approx. 10 µL or methanol standard (5 or 10 mg water/mL). References: G. Wieland, Water determination by Karl Fischer Titration, GIT Verlag, Darmstadt, Germany HYDRANAL® Practical Course, Water reagents for Karl-Fischer-Titration according to Eugen Scholz, Riedel de Haën, Seelze, Germany METROHM Application Bulletin No. 77: Karl Fischer Water Determinations – Result in mg/mL – Sample size in g – Factor The factor depends on type and water content of the standard: Standard used Sample size in water water methanol methanol methanol g µL g mL µL Factor 1000 density (H2O) = 1 g/mL water content in mg/g water content in mg/mL 0.001 ∗ water content in mg/mL C39 is the common variable for the titer 795 KFT Titrino 6.3 User methods 6.3.3 KF Titer determination with sodium tartrate "TarTiter" 'pa 795 KFT Titrino 795.0010 date 2001-11-15 time 14:56 0 KFT Ipol TarTiter parameters >control parameters EP at U 250 mV dynamics 100 mV max.rate max. ml/min min.volume incr. min. µl stop crit: drift stop drift 20 µl/min >titration parameters titr.direction: pause 1 0 s start V: OFF pause 2 0 s extr.time 0 s I(pol) 50 µA electrode test: OFF temperature 25.0 °C time interval 2 s >stop conditions stop V: abs. stop V 99.99 ml filling rate max. ml/min >statistics status: ON mean n= 5 res.tab: original >preselections conditioning: ON display drift: ON drift corr: OFF req.ident: OFF req.smpl size: value limit smpl size: OFF oven: no activate pulse: OFF -----------'fm 795 KFT Titrino 795.0010 date 2001-11-15 time 14:56 0 KFT Ipol TarTiter >calculations Titer=C00/EP1*C01;4;mg/ml C00= 1.0 C01= 156.6 -----------'de 795 KFT Titrino 795.0010 date 2001-11-15 time 14:56 KFT Ipol TarTiter def >formula Titer=C00/EP1*C01 RS1 text Titer RS1 decimal places 4 RS1 unit: mg/ml RS1 limit control: OFF >silo calculations match id: OFF >common variables C39=MN1 >report report COM1:full; >mean MN1=RS1 >temporary variables ------------ 795 KFT Titrino The titer is calculated as mean value out of 5 single determinations and stored as common variable C39. Therefore, it can be directly used in subsequent methods. Electrode: Double Pt-electrode 6.0338.100 at measuring input "Pol". Titrating agent: One-component or two-component KarlFischer reagent, ready to use. Solvent: 20 mL Methanol or a specific solvent, conditioned. Sample: 200–300 mg Disodium tartrate dihydrate (water content 15.66 ±0.05%), stir to complete dissolution. References: G. Wieland, Water determination by Karl Fischer Titration, GIT Verlag, Darmstadt, Germany HYDRANAL® Practical Course, Water reagents for Karl-Fischer-Titration according to Eugen Scholz, Riedel de Haën, Seelze, Germany METROHM Application Bulletin No. 77: Karl Fischer Water Determinations – Result in mg/mL – Sample size in g – Water content of disodium tartrate dihydrate ∗ 10 If the sample size is given in mg, the factor is 0.1566. C39 is the common variable for the titer 131 6.3 User methods 6.3.4 Blank determination for KFT "Blank_KF" 'pa 795 KFT Titrino 795.0010 date 2001-11-15 time 18:01 0 KFT Ipol Blank_KF parameters >control parameters EP at U 250 mV dynamics 100 mV max.rate max. ml/min min.volume incr. min. µl stop crit: drift stop drift 20 µl/min >titration parameters titr.direction: pause 1 0 s start V: OFF pause 2 0 s extr.time 0 s I(pol) 50 µA electrode test: OFF temperature 25.0 °C time interval 2 s >stop conditions stop V: abs. stop V 99.99 ml filling rate max. ml/min >statistics status: ON mean n= 3 res.tab: original >preselections conditioning: ON display drift: ON drift corr: OFF req.ident: OFF req.smpl size: OFF limit smpl size: OFF oven: no activate pulse: OFF -----------'fm 795 KFT Titrino 795.0010 date 2001-11-15 time 18:01 0 KFT Ipol Blank_KF >calculations Blank=EP1;4;ml -----------'de 795 KFT Titrino 795.0010 date 2001-11-15 time 18:02 KFT Ipol Blank_KF def >formula Blank=EP1 RS1 text Blank RS1 decimal places 4 RS1 unit: ml RS1 limit control: OFF >silo calculations match id: OFF >common variables C38=MN1 >report report COM1:full; >mean MN1=RS1 >temporary variables ------------ 132 This method can be generally used for KF blank determinations. For work with a KF oven, you need to enter an extraction time in key <PARAM>, ">titration parameters". The mean value out of 3 determinations is assigned to the common variable C38. Electrode: Double Pt-electrode 6.0338.100 at measuring input "Pol". Titrating agent: One-component or two-component KarlFischer reagent, ready to use. Solvent: 20 mL Methanol or a specific solvent, conditioned. Sample: E.g. 1.000 mL methanol (as used for extraction) or another solvent. References: G. Wieland, Water determination by Karl Fischer Titration, GIT Verlag, Darmstadt, Germany HYDRANAL® Practical Course, Water reagents for Karl-Fischer-Titration according to Eugen Scholz, Riedel de Haën, Seelze, Germany METROHM Application Bulletin No. 77: Karl Fischer Water Determinations C38 is the common variable for the KF blank value. 795 KFT Titrino 6.3 User methods 6.3.5 KF-titration with blank value subtraction "KF-Blank" 'pa 795 KFT Titrino 795.0010 date 2001-11-15 time 18:04 0 KFT Ipol KF-Blank parameters >control parameters EP at U 250 mV dynamics 100 mV max.rate max. ml/min min.volume incr. min. µl stop crit: drift stop drift 20 µl/min >titration parameters titr.direction: pause 1 0 s start V: OFF pause 2 0 s extr.time 0 s I(pol) 50 µA electrode test: OFF temperature 25.0 °C time interval 2 s >stop conditions stop V: abs. stop V 99.99 ml filling rate max. ml/min >statistics status: ON mean n= 3 res.tab: original >preselections conditioning: ON display drift: ON drift corr: OFF req.ident: OFF req.smpl size: all limit smpl size: OFF oven: no activate pulse: OFF -----------'fm 795 KFT Titrino 795.0010 date 2001-11-15 time 18:04 0 KFT Ipol KF-Blank >calculations Water=(EP1-C38)*C39*C01/C00/C02;2;% Titer=C39;4;mg/ml Blank=C38;4;ml C00= 1.0 C01= 0.1 C02= 1 C38= 0.0 C39= 0.0 ------------ 795 KFT Titrino KF-titration regarding a blank value (e.g. for an extraction solvent), being determined before and stored as common variable C38 (see page 132). For work with a KF oven, you need to enter an extraction time in key <PARAM>, ">titration parameters". Electrode: Double Pt-electrode 6.0338.100 at measuring input "Pol". Titrating agent: One-component or two-component KarlFischer reagent, ready to use. Solvent: 20 mL Methanol or a specific solvent, conditioned. Sample: Sample size depending on expected consumption of KF reagent. References: G. Wieland, Water determination by Karl Fischer Titration, GIT Verlag, Darmstadt, Germany HYDRANAL® Practical Course, Water reagents for Karl-Fischer-Titration according to Eugen Scholz, Riedel de Haën, Seelze, Germany METROHM Application Bulletin No. 77: Karl Fischer Water Determinations – Result in % – Sample size in g – Factor for % (see page 134) – Divisor (see page 134) – Blank value in mL – KF titer 133 6.3 User methods 'de 795 KFT Titrino 795.0010 date 2001-11-15 time 18:04 KFT Ipol KF-Blank def >formula Water=(EP1-C38)*C39*C01/C00/C02 RS1 text Water RS1 decimal places 2 RS1 unit: % RS1 limit control: OFF Titer=C39 RS2 text Titer RS2 decimal places 4 RS2 unit: mg/ml RS2 limit control: OFF Blank=C38 RS3 text Blank RS3 decimal places 4 RS3 unit: ml RS3 limit control: OFF >silo calculations match id: OFF >common variables >report report COM1:full; >mean MN1=RS1 >temporary variables ------------ Adjust the calculation values C01 and C02 according the desired result unit and your sample size. Unit RS % % % ppm ppm ppm mg/mL mg/mL g/L g/L mg mL mg/pc 134 Sample size in.. g mg mL g mL µL g mL g mL 1 1 pc C01 0.1 100 0.1 1000 1000 1000 000 Density of Sample 1 Density of Sample 1 1 1 1 C02 1 1 Density of Sample 1 Density of Sample Density of Sample 1 1 1 1 1 1000 ∗ Density H2O 1 795 KFT Titrino 6.3 User methods 6.3.6 KF-titration without blank value subtraction "KF" 'pa 795 KFT Titrino 795.0010 date 2001-11-15 time 18:06 0 KFT Ipol KF parameters >control parameters EP at U 250 mV dynamics 100 mV max.rate max. ml/min min.volume incr. min. µl stop crit: drift stop drift 20 µl/min >titration parameters titr.direction: pause 1 0 s start V: OFF pause 2 0 s extr.time 0 s I(pol) 50 µA electrode test: OFF temperature 25.0 °C time interval 2 s >stop conditions stop V: abs. stop V 99.99 ml filling rate max. ml/min >statistics status: ON mean n= 3 res.tab: original >preselections conditioning: ON display drift: ON drift corr: OFF req.ident: OFF req.smpl size: all limit smpl size: OFF oven: no activate pulse: OFF -----------'fm 795 KFT Titrino 795.0010 date 2001-11-15 time 18:06 0 KFT Ipol KF >calculations Water=EP1*C39*C01/C00/C02;2;% Titer=C39;4;mg/ml C00= 1.0 C01= 0.1 C02= 1 C39= 0.0 ------------ 795 KFT Titrino KF titration without blank value subtraction. Electrode: Double Pt-electrode 6.0338.100 at measuring input "Pol". Titrating agent: One-component or two-componenet KarlFischer reagent, ready to use. Solvent: 20 mL Methanol or a specific solvent, conditioned. Sample: Sample size depending on expected consumption of KF reagent. References: G. Wieland, Water determination by Karl Fischer Titration, GIT Verlag, Darmstadt, Germany HYDRANAL® Practical Course, Water reagents for Karl-Fischer-Titration according to Eugen Scholz, Riedel de Haën, Seelze, Germany METROHM Application Bulletin No. 77: Karl Fischer Water Determinations – Result in % – Sample size in g – Factor for % (see page 134) – Divisor (see page 134) – KF titer 135 6.3 User methods 'de 795 KFT Titrino 795.0010 date 2001-11-15 time 18:06 KFT Ipol KF def >formula Water=EP1*C39*C01/C00/C02 RS1 text Water RS1 decimal places 2 RS1 unit: % RS1 limit control: OFF Titer=C39 RS2 text Titer RS2 decimal places 4 RS2 unit: mg/ml RS2 limit control: OFF >silo calculations match id: OFF >common variables >report report COM1:full; >mean MN1=RS1 >temporary variables ------------ 136 795 KFT Titrino 6.3 User methods 6.3.7 KF titrations with various KF reagents If you work parallel with different KF reagents, you can use different methods for each KF reagent. The titer determination is performed with H2O or methanol standard as described for the method "H2OTiter". The factor C01 has to be adapted to the standard used (see page 130). For each reagent, the titer is assigned to another common variable which is taken into account in the calculations of the titration method (see table). The titration parameters are suitable both for water determinations using one-component reagents and two-component reagents. The KF titations without blank value subtraction are executed according to the description for the method "KF" (see page 135). For the blank determination the method "Blank_KF" is used. The mean value of three blank determinations is assigned to the common variable C38. The KF titations with blank value subtraction are executed according to the description for the method "KF-Blank " (see page 133). Remember that you need to adapt the factors in the formula (see table on page 134). KF reagents Methods One-component- or twocomponent KF reagent (5 mg/mL H2O) for medium and high amounts of water Titer determination KF-titration without BV-subtr. KF-titration with BV-subtraction Blank determination 5Titer 5Deter 5Deter-B Blank_KF Titer = C32 Calculation with C32 Calculation with C32 and C38 Blank = C38 One-component- or twocomponent KF reagent (2 mg/mL H2O) for small amounts of water Titer determination 2Titer KF-titration without BV-subtr. 2Deter KF-titration with BV-subtraction 2Deter-B Titer = C33 Calculation with C33 Calculation with C33 and C38 Blank = C38 Blank determination Common Variables Blank_KF One-component- or twocomponent KF reagent (1 mg/mL H2O) for micro-determination of water Titer determination 1Titer KF-titration without BV-subtr. 1Deter KF-titration with BV-subtraction 1Deter-B Special KF reagent for water determination in solutions that contain aldehydes and/or ketones Titer determination KetTiter KF-titration without BV-subtr. KetDeter KF-titration with BV-subtraction KetDet-B Blank determination Blank determination Blank_KF Blank_KF Titer = C34 Calculation with C34 Calculation with C34 and C38 Blank = C38 Titer = C35 Calculation with C35 Calculation with C35 and C38 Blank = C38 BV = Blank value If you use various titration reagents, generally make sure that the values of the titers for the various titration reagents are assigned to different common variables which are taken into account in the calculations of the corresponding titration methods. 795 KFT Titrino 137 6.3 User methods 6.3.8 Determination of the bromine number "BrNumber" 'pa 795 KFT Titrino 795.0010 date 2001-11-15 time 14:52 0 KFT Ipol BrNumber parameters >control parameters EP at U 500 mV dynamics 500 mV max.rate 5 ml/min min.volume incr. min. µl stop crit: time t(delay) 30 s >titration parameters titr.direction: pause 1 0 s start V: OFF pause 2 0 s extr.time 0 s I(pol) 10 µA electrode test: OFF temperature 25.0 °C time interval 2 s >stop conditions stop V: abs. stop V 99.99 ml filling rate max. ml/min >statistics status: ON mean n= 3 res.tab: original >preselections conditioning: OFF req.ident: OFF req.smpl size: value limit smpl size: OFF activate pulse: OFF -----------'fm 795 KFT Titrino 795.0010 date 2001-11-15 time 14:52 0 KFT Ipol BrNumber >calculations BrNumber=(EP1-C01)*C02*C03*C04/C00;0; C00= 1.0 C01= 0.0 C02= 0.5 C03= 7.99 C04= 100 -----------'de 795 KFT Titrino 795.0010 date 2001-11-15 time 14:52 KFT Ipol BrNumber def >formula BrNumber=(EP1-C01)*C02*C03*C04/C00 RS1 text BrNumber RS1 decimal places 0 RS1 unit: RS1 limit control: OFF >silo calculations match id: OFF >common variables >report report COM1:full; >mean MN1=RS1 >temporary variables ------------ 138 Determination of the bromine number in petroleum hydrocarbons according to ASTM D 1159-84. The bromine number is defined as the quantity of bromine in mg which reacts with 100 g of the sample. Electrode: Double Pt-electrode 6.0338.100 at measuring input "Pol". Titrating agent: Bromide/bromate-solution, c(BrO3–/Br–) = 0.5 mol/L Dissolve 51.0 g KBr and 13.92 g KBrO3 each in distilled water and add up to 1 L. Solvent: 714 mL glacial acetic acid, 134 mL 1,1,1-trichlorethane, 134 mL methanol, 18 mL w(H2SO4) = 0.2 (20%) Sample: Pipet 25 mL 1,1,1-Trichloroethane into a 50-mL volumetric flask and add the sample (see table below). The weight of the sample is obtained by difference between the weight of the flask before and after addition of the sample. Fill the flask to the mark with 1,1,1-trichloroethane and mix well. Add 5 mL of the sample solution to 110 mL solvent in the titration vessel and mix. The blank sample is titrated in the same way. – Result in % (g bromine/100 g sample) – Sample size in g – Consumption of Blank sample in mL – Normality of the titrating agent in mol/L – Molecular mass of Br (79.9 g/mol) ∗ 0.1 (Conversion to % in weight and L) – C04 = Dilution factor (Has to be calculated ac cording to the sample preparation, for the method described above, the factor is 10.) Bromine no. (%, w/w) Sample size (g) 0...10 20...16 10...20 10...8 20...50 5...4 50...100 2...1.5 100...200 1.0...0.5 References: ASTM D 1159-84 Metrohm Application Bulletin No. 177 795 KFT Titrino 6.4 Titrino validation 6.4 Titrino validation Checking and maintenance of the Titrino is carried out in 3 steps: 1. Testing the electronic components when the Titrino is switched on. 2. Wet-chemistry validation of the whole analysis setup 3. Maintenance and adjustment of the Titrino by Metrohm service. 6.4.1 Electronic tests When the Titrino is switched on electronic tests are carried out. During this period system appears in the display. The tests are documented in the system test report, which can be printed out when the Titrino is switched on (see page 10): tests 'di 795 KFT Titrino 01103 date time 2001-11-15 RAM test OK real time clock OK timer OK A/D converter OK LCD display OK COMPorts OK EPROM test 795.0010 07:24 Contact Metrohm service if one of these tests is "not OK". If the "real time clock" test is not ok, you can try to set date and time again. If the test is OK afterwards you should check whether your stored methods have remained unchanged. OK ============ 6.4.2 Wet tests GLP (Good Laboratory Practice) requires the periodic validation of the analytical instruments. The reproducibility and accuracy of the instruments are checked. An annual repetition of the procedure appears to be sensible. Depending on the requirements a more frequent check may be indicated, e.g. every 3 or 6 months. Guidelines for the testing regulations (SOP, Standard Operating Procedure) are given in Metrohm Application Bulletin No. 255: Validation of Metrohm KF Titrators and KF Oven according to GLP/ISO 9001. The validation interval can be checked by the Titrino (set under <CONFIG>, monitoring). If the interval has elapsed the Titrino displays the message validate instrument. 6.4.3 Maintenance and adjustment of the Titrino The Titrino should be serviced and adjusted by Metrohm service at regular intervals. The Titrino can check the date of the next service with the help of the monitoring function "Service" under <CONFIG>, monitoring. If this date has been passed then the Titrino will display the message service is due. 795 KFT Titrino 139 6.5 Warranty and conformity 6.5 Warranty and conformity 6.5.1 Warranty The warranty regarding our products is limited to rectification free of charge in our workshops of defects that can be proved to be due to material, design or manufacturing faults which appear within 12 months from the day of delivery. Transport costs are chargeable to the purchaser. For day and night operation, the warranty is valid for 6 months. Glass breakage in the case of electrodes or other glass parts is not covered by the warranty. Checks which are not a result of material or manufacturing faults are also charged during the warranty period. For parts of outside manufacture insofar as these constitute an appreciable part of our instrument, the warranty stipulations of the manufacturer in question apply. With regard to the guarantee of accuracy, the technical specifications in the Instructions for Use are authoritative. Concerning defects in material, construction or design as well as the absence of guaranteed features, the purchaser has no rights or claims except those mentioned above. If damage of the packaging is evident on receipt of a consignment or if the goods show signs of transport damage after unpacking, the carrier must be informed immediately and a written damage report demanded. Lack of an official damage report releases METROHM from any liability to pay compensation. If any instruments and parts have to be returned, the original packaging should be used if at all possible. This applies above all to instruments, electrodes, buret cylinders and PTFE pistons. Before embedment in wood shavings or similar material, the parts must be packed in a dustproof package (for instruments, use of a plastic bag is imperative). If open assemblies are enclosed in the scope of delivery that are sensitive to electromagnetic voltages (e.g. data interfaces etc.) these must be returned in the associated original protective packaging (e.g. conductive protective bag). (Exception: assemblies with built-in voltage source belong in a non-conductive protective packaging). For damage which arises as a result of noncompliance with these instructions, no warranty responsibility whatsoever will be accepted by METROHM. 140 795 KFT Titrino 6.5 Warranty and conformity 6.5.2 EU Declaration of conformity EU Declaration of Conformity The company Metrohm AG, Herisau, Switzerland, certifies herewith, that the following instrument: 795 KFT Titrino meets the CE mark requirements of EU Directives 89/336/EWG and 73/23/EWG. Source of specifications: EN 50081 EN 50082 EN 61010 Electromagnetic compatibility — Generic emission standard Electromagnetic compatibility — Generic immunity standard Safety requirements for electrical equipment for measurement, control and laboratory use Description of apparatus: Titrator for fast and precise water determination with LCD graphical display. Titration sequences can be programmed and methods stored in the internal memory. Herisau, October 30, 2001 795 KFT Titrino Dr. J. Frank Ch. Buchmann Development Manager Production and Quality Assurance Manager 141 6.5 Warranty and conformity 6.5.3 Certificate of Conformity and System Validation Certificate of Conformity and System Validation This is to certify the conformity to the standard specifications for electrical appliances and accessories, as well as to the standard specifications for security and to system validation issued by the manufacturing company. Name of commodity: 795 KFT Titrino System software: Stored in ROMs Name of manufacturer: Metrohm Ltd., Herisau, Switzerland This Metrohm instrument has been built and has undergone final type testing according to the standards: Electromagnetic compatibility: IEC61326-1 Electromagnetic compatibility: Emission EN50081-1, EN50081-2, EN55022 (class B), IEC61000-3-2 Electromagnetic compatibility: Immunity EN50082-1, IEC61000-6-2, Namur, IEC61000-4-2, IEC61000-4-3, ENV50204, IEC61000-4-4, IEC61000-4-5, IEC61000-4-6, IEC61000-4-11 Safety specifications IEC61010-1, EN61010-1, UL3101-1 It has also been certified by the Swiss Electrotechnical Association (SEV), which is member of the International Certification Body (CB/IEC). The technical specifications are documented in the instruction manual. The system software, stored in Read Only Memories (ROMs) has been validated in connection with standard operating procedures in respect to functionality and performance. The features of the system software are documented in the instruction manual. Metrohm Ltd. is holder of the SQS-certificate of the quality system ISO 9001 for quality assurance in design/development, production, installation and servicing. Herisau, October 30, 2001 142 Dr. J. Frank Ch. Buchmann Development Manager Production and Quality Assurance Manager 795 KFT Titrino 6.6 Scope of delivery and ordering designations 6.6 Scope of delivery and ordering designations 795 KFT Titrino ......................................................................................2.795.0010 inclusive the following accessories: 1 Keypad for KFT Titrino 795 ................................................................................ 6.2130.070 1 Key for Exchange Units ..................................................................................... 6.2739.010 1 Double Pt-electrode with plug-in head, without cable....................................... 6.0338.100 1 Electrode cable with plug F 1M ......................................................................... 6.2104.020 1 Titration vessel lid .............................................................................................. 6.1414.030 1 Titration vessel 20 mL........................................................................................ 6.1415.220 1 Titration vessel 50 mL........................................................................................ 6.1415.250 1 Set of O-rings for the Titration vessel lid............................................................ 6.1244.040 1 Drying tube ........................................................................................................ 6.1403.040 1 Molecular sieve 250 g........................................................................................ 6.2811.000 2 Screw nipple for KF ........................................................................................... 6.2730.010 1 Stopper with septum, diameter 18 mm ............................................................. 6.2730.020 3 Stopper with nipple and O-ring ......................................................................... 6.2730.030 2 Septum (5 p.)..................................................................................................... 6.1448.010 1 Glass weighing spoon....................................................................................... 6.2412.000 2 Teflon stirring bar, length 16 mm....................................................................... 6.1903.020 2 Teflon stirring bar, length 25 mm....................................................................... 6.1903.030 1 Cover ................................................................................................................. 6.2723.130 1 Mains cable with cable socket, type CEE(22), V Cable plug to customer's specifications type SEV 12 (Switzerland...)............................................................................. 6.2122.020 type CEE(7), VII (Germany...)........................................................................... 6.2122.040 type NEMA/ASA (USA...) ................................................................................. 6.2122.070 1 Vesuv 3.0 light, PC program for data acquisition and method backup for 2 devices .................................................................................................. 6.6008.500 1 Instructions for Use for 795 KFT Titrino ............................................................. 8.795.1003 1 Quick References for 795 KFT Titrino................................................................ 8.795.1013 1 Short Operating Guide for 795 KFT Titrino ........................................................ 8.795.1023 795 KFT Titrino 143 6.6 Scope of delivery and ordering designations Options Accessories to separate order and on payment of extra charge: Burets Auxiliary burets 765 Dosimat ......................................................................................................... 2.765.0010 776 Dosimat ......................................................................................................... 2.776.0010 Cable 795 KFT Titrino (activate pulse, line L6) — 765 or 776 Dosimat ............... 6.2139.000 Exchange Units V = 1 mL ........................................................................................................ 6.3026.110 V = 5 mL ........................................................................................................ 6.3026.150 V = 10 mL ........................................................................................................ 6.3026.210 V = 20 mL ........................................................................................................ 6.3026.220 V = 50 mL ........................................................................................................ 6.3026.250 Stirrers and Titrating Stands 703 Ti Stand for KF titrations................................................................................ 2.703.0010 728 Magnetic stirrer.............................................................................................. 2.728.0040 727 Ti Stand for rinsing and addition of fresh solvent.......................................... 2.727.0010 802 Rod Stirrer ..................................................................................................... 2.802.0010 727 Ti Stand with built-in magnetic stirrer ............................................................ 2.727.0100 Titration equipment Equipment for KF titrations .................................................................................6.5609.000 Titration vessel, volumes 1... 50 mL ...................................................................................................6.1415.110 5... 70 mL ...................................................................................................6.1415.150 10... 90 mL, order 6.2036.000 holding ring separately ................................6.1415.210 20... 90 mL ...................................................................................................6.1415.220 50... 150 mL ...................................................................................................6.1415.250 70... 200 mL ...................................................................................................6.1415.310 Titration vessel with thermostatic jacket, volumes 1... 50 mL ...................................................................................................6.1418.110 5... 70 mL ...................................................................................................6.1418.150 20... 90 mL ...................................................................................................6.1418.220 50... 150 mL ...................................................................................................6.1418.250 Titration vessel lid (5 openings) ..........................................................................6.1414.010 Magnetic stirring bars, length 12 mm............................................................................................................6.1903.010 16 mm............................................................................................................6.1903.020 25 mm............................................................................................................6.1903.030 Electrode holder ..................................................................................................6.2021.020 144 795 KFT Titrino 6.6 Scope of delivery and ordering designations Electrodes and accessories Double Pt-electrode with plug-in head, without cable ....................................... 6.0338.100 Electrode cable, 1m ........................................................................................... 6.2104.020 Printers Printer Custom DP40-S4N.................................................................................... 2.140.0200 Cable Titrino – Custom DP40-S4N ....................................................................... 6.2134.110 Cable Titrino – Seiko DPU-414 ............................................................................. 6.2134.110 Cable Titrino – EPSON LX300+ (9/25 pins) ........................................................ 6.2134.050 Cable Titrino – HP Desk Jet (serial interface) (9/25 pins)..................................... 6.2134.050 Cable Titrino – HP Desk/Laser Jet (parallel IF)..................................................... 2.145.0330 Adapter for connection of printer/balance at the same COM ......... 6.2125.010+6.2125.030 Balance For Mettler cables you need an adapter 9/25 pins .............................................. 6.2125.010 Cable Sartorius – balances MP8, MC1 (9/25 pins) .............................................. 6.2134.060 Cable Shimadzu – balances BX, BW .............................................. 6.2125.080+6.2125.010 Ohaus Voyager, Explorer, Analytical Plus balances.................................. cable from Ohaus Mettler AB, AG balances (interface LC-RS25)..........................................cable with balance Mettler AT balance ....................................................................... 6.2146.020+6.2125.010 Mettler AM, PM balance ....................... 6.2146.020+6.2125.010+accessories from Mettler Mettler balances with interface 016 ...........................................................cable from Mettler Mettler balances with interface 011 or 012...................................... 6.2125.020+6.2125.010 Mettler PG, AB-S................................................................................................... 6.2134.110 Mettler AX, MX, UMX ............................................................................................ 6.2134.120 AND balances (with RS232 interface OP-03) .................................. 6.2125.020+6.2125.010 Precisa balances ............................................................................. 6.2125.080+6.2125.010 Adapter for connection of printer/balance at the same COM ......... 6.2125.010+6.2125.030 Connection of PC keyboard and/or barcode reader Remote Box .......................................................................................................... 6.2148.000 Connection of 768 KF Oven KF Oven................................................................................................................ 2.768.0010 Cable 795 KFT Titrino — 768 KF Oven, control ................................................... 6.2141.010 Cable 795 KFT Titrino — 768 KF Oven, data ....................................................... 6.2125.110 PC connection Cable 795 KFT Titrino – PC (9 pins female / 9 pins female)................................. 6.2134.040 Cable 795 KFT Titrino – PC (9 pins female / 25 pins female)............................... 6.2125.110 RS232 C extension cable (25 pins male / 25 pins female)................................... 6.2125.020 RS232 C extension cable (9 pins male / 9 pins female)...................................... 6.2134.110 Vesuv 3.0, PC program for data acquisition and method backup for up to 64 devices....................................................................................... 6.6008.200 795 KFT Titrino 145 6.6 Scope of delivery and ordering designations Sample Changer 730 Sample Changer, 1 working station, 1 pump and 2 stirrer connections....... 2.730.0010 730 Sample Changer, 1 working station, 2 pumps and 2 stirrer connections..... 2.730.0020 730 Sample Changer, 1 working station, no pumps and 2 stirrer connections... 2.730.0030 730 Sample Changer, 2 working stations, 2 pumps and 4 stirrer connections ... 2.730.0110 730 Sample Changer, 2 working stations, 4 pumps and 4 stirrer connections ... 2.730.0120 730 Sample Changer, 2 working stations, no pumps and 4 stirrer connections. 2.730.0130 760 Sample Changer, 1 working station, no pumps and 2 stirrer connections... 2.760.0020 for KFT applications 774 Oven Sample Processor ............................................................................... 2.774.0010 Cable 795 KFT Titrino — 730, 760, 774 Sample Changer ................................... 6.2141.020 Cable 2x 795 KFT Titrino — 730, 760 Sample Changer ...................................... 6.2141.030 Cable Titrino — 730, 760 Sample Changer+665, 725, 765, 776 Dosimat ......... 6.2141.040 Cable Titrino — 730, 760 Sample Changer+ 2x 665, 725, 765, 776 Dosimat ... 6.2141.050 Cable 795 KFT Titrino — Control Unit 664 for Sample Changer 673/674 ........... 3.980.3560 146 795 KFT Titrino Index Index Keys are marked with < >, display green part are printed in italic. texts are in bold characters, and pages concerning the A <ABC> .......................................................8 Accessories ...........................................143ff activate pulse: ........................................19 Analog potentiometer..................................3 Automatic reports ......................................31 auto start .................................................11 auxiliaries ...............................................11 B balance: ....................................................10 Balance connection.................................114 barcode: ....................................................11 Barcode reader .................................11, 118 baud rate: .................................................12 bytes missing ...........................................97 C Cables ...................................................145ff Calculations...............................................25 Certificates...............................................141 CE ............................................................141 <C-FMLA> ...........................................6, 27 Characters input ..........................................8 check ......................................................97 <CLEAR> ...................................................6 common variables ................................12, 30 Computer connection..............................118 COM X characteristics .................................... 90ff configuration ........................................12 pin assignment ....................................93 conditioning: ...........................................18 <CONFIG>.............................................6, 9 Configuration ...............................................9 Conformity ...............................................140 Connection balance ..............................................114 barcode reader ..................................118 computer............................................118 electrode ............................................122 Karl Fischer oven ...............................115 oven sample processor .....................117 PC keyboard ......................................119 printer .................................................113 remote box .........................................118 sample changer .................................116 stirrer ..................................................112 Ti Stand ..............................................112 795 KFT Titrino Connection cables ................................ 145ff Contrast of display ...................................... 3 control parameters .................................. 15 Control parameters KFT ........................... 21 Cursor keys ................................................. 6 curve ......................................................... 13 <CURVE> ................................................ 33 Curve changing output .................................. 15 display.................................................. 33 examples ............................................. 32 printing ................................................. 31 cycle lines: ............................................. 40 D data bit: .................................................. 12 Data input ................................................... 7, 8 output................................................... 31 reproduction ........................................ 32 transfer (RS232)................................. 45ff date ........................................................... 11 Decimal places ......................................... 26 <DEF> ............................................... 6, 25ff delete all:............................................... 40 delete all silo lines ............................ 40 delete line n ........................................... 39 delete n .................................................... 28 Delete common variables ............................... 30 formulas ............................................... 25 methods............................................... 36 statistic values ..................................... 28 text ......................................................... 8 user name............................................ 34 delete silo lines .................................... 39 dev.label .................................................. 11 Diagnosis .............................................. 100ff Diagnosis report...................................... 139 dialog: ...................................................... 11 Display, contrast ......................................... 3 display drift: ......................................... 18 division by zero ..................................... 97 <DOS> ................................................ 3, 44 Dosing ................................................... 3, 44 dos.rate .................................................... 17 drift corr:............................................... 18 drift value............................................... 18 dynamics .................................................... 15 147 Index E edit silo lines ....................................... 39 electrode test: ....................................... 17 <ENTER>................................................... 6 Entry of data ........................................................ 7 text.......................................................... 8 EP at.......................................................... 15 Error messages............................... 49ff, 97ff error XX .................................................... 97 Exchange Unit ......................................... 144 extr.time .................................................. 17 F Fabrication number..................................... 5 factor .................................................. 17, 18 Filling rate after determination............................... 18 after manual dosing............................... 3 formula ...................................................... 25 G General rules for RS232.......................... 45ff GLP.......................................................... 139 Graphics changing output .................................. 13 display.................................................. 33 examples.............................................. 32 printing ................................................. 31 H ................................................ 12 Handshake................................................ 90 Hardware handshake................................ 93 handshake: I id#1 or C21 ......................................... 37, 39 Identification ........................................ 37, 39 request ................................................. 18 Initialize RAM ........................................... 110 Input of values..................................................... 7 text.......................................................... 8 Inquiries....................................................... 7 I/O lines ................................................... 125 I(pol) ........................................................ 17 ISO........................................................... 142 K Karl Fischer oven .............................. 19, 115 Karl Fischer titration ................................ 15ff keyboard: .................................................. 10 Keycode .................................................. 102 Keypad ........................................................ 6 148 Keys ............................................................ 6 <ABC> ................................................. 8 <C-FMLA> ......................................... 27 <CLEAR> ............................................. 6 <CONFIG>........................................... 9 <CURVE> .......................................... 33 <DEF>.............................................. 25ff <DOS>................................................. 3 <ENTER>............................................. 6 <MEAS/HOLD> ................................... 6 <MODE>............................................ 14 <PARAM> ........................................ 15ff <PRINT> ...................................... 32, 33 <QUIT> ................................................ 6 <REPORTS> ...................................... 32 <SILO>............................................... 38 <SMPL DATA>................................. 37ff <START> ............................................. 6 <STATISTICS>............................... 3, 29 <STOP> ............................................... 6 <USER> ............................................. 34 <USER METH>.................................. 35 KFT.......................................................... 15ff L Language.................................................. 11 LED ....................................................... 3, 29 Limit control result .................................................... 26 sample size ......................................... 19 limit smpl size: ..................................... 19 Lock functions........................................... 12 low lim. .................................................... 19 M Mains .................................................. 5, 112 Malfunctions.......................... 49ff, 97ff, 100ff man.reports to COM: ................................ 10 Manual operation...................................... 6ff manual stop .............................................. 98 match id: .................................................. 42 max.rate .................................................... 16 mean n ....................................................... 28 Mean values calculation ........................................... 28 delete results ....................................... 28 report ................................................... 42 silo ....................................................... 43 <MEAS/HOLD>......................................... 6 meas.pt list overflow ............................ 98 measured quantity:.................................. 14 Measuring point list printing ..................... 31 Method................................................ 35, 39 method name: ............................................ 35 min.volume incr. ..................................... 16 missing EP ................................................ 98 795 KFT Titrino Index <MODE>..................................................14 Mode KFT ..................................................15 monitoring ...................................................9 N name: ..........................................................34 next service: .............................................9 no... ..........................................................98 not valid...................................................98 O Object tree............................................... 52ff Ordering designations.............................143 Outputs..................................................125ff Oven ..................................................19, 115 Overview ......................................................2 P Parameters KFT.........................................15 <PARAM> ..........................................6, 15ff parity: ......................................................12 pause (X).............................................16, 17 peripheral units ......................................10 Pin assignment "Remote" socket .................................125 RS232...................................................93 Power connection................................5, 112 preselections ...........................................18 <PRINT> ..............................................6, 33 Printing.....................................................31ff Printer connection .........................................113 problems ..............................................95 selection ...............................................10 Problems KF titrations ..........................................24 printer ...................................................95 program ......................................................11 Q <QUIT> ......................................................6 R RAM, initialize ..........................................110 recall method ...........................................35 remote box: ...............................................10 Remote control via "Remote" lines...............................125 via RS232 ........................................... 45ff Remote control commands detailed description ........................... 67ff overview ...............................................52 report COMX: .............................................31 Report 795 KFT Titrino output................................................. 31ff printing ................................................. 31 reproduction ........................................ 32 selection............................................... 31 <REPORTS>............................................ 32 req.ident: ................................................ 18 req.smpl size: ......................................... 19 res.tab: .................................................... 28 Result calculation............................................ 25 delete ................................................... 28 display.................................................. 11 limit control........................................... 26 report.................................................... 31 store ............................................... 40, 41 text ....................................................... 26 result display: ....................................... 11 RS1 decimal places .................................. 26 RS1 L13 output: ....................................... 26 RS1 limit control: .................................. 26 RS1 low lim. ............................................. 26 result out of limits .............................. 98 RS1 text .................................................... 26 RS1 unit: .................................................. 26 RS1 up lim................................................ 26 RS232 settings COMX ................................ 12 RS232 interface characteristics.................................... 90ff configuration ........................................ 12 pin assignment .................................... 93 run number ................................................ 11 S Sample addition ........................................ 23 Sample changer...................................... 116 Sample data............................................ 37ff Sample identification................................. 37 inquiry .................................................. 18 Sample size......................................... 37–39 limit control........................................... 19 sample size out ....................................... 98 save lines:............................................... 40 Scope of delivery .................................... 143 Selection of balance ................................................ 10 printer................................................... 10 send to COMX: ........................................... 10 Sequence KFT .......................................... 20 Serial number .............................................. 5 service: .................................................... 10 service is due ......................................... 98 Setting up .............................................. 112ff <SILO> ................................................ 6, 38 silo calculations .............................. 41, 42 silo empty ................................................ 98 silo full .................................................. 98 149 Index ................................................ 39 Silo reports .......................................... 31, 43 <SMPL DATA> .................................. 6, 37ff smpl size ............................................ 37, 39 smpl unit: .......................................... 37, 39 Software handshake ................................. 90 Special messages..................................... 97 <START> ................................................... 6 start delay ............................................... 11 start V ...................................................... 17 Start volume .............................................. 17 <STATISTICS>..................................... 6, 28 statistics ................................................ 28 Statistics calculations................................ 28 Statistics values delete results........................................ 28 report.................................................... 31 silo........................................................ 42 Stirrer connection .................................... 112 stirrer control:...................................... 10 <STOP>..................................................... 6 stop bit: .................................................. 12 stop conditions ....................................... 18 stop crit: ................................................ 16 Stop criterion ............................................. 16 stop drift ................................................ 16 stop V reached ......................................... 99 stop time .................................................. 16 stop V ........................................................ 18 Store methods............................................... 35 results............................................. 41, 42 Survey.......................................................... 2 system error XX ....................................... 99 system test report: ................................ 10 silo lines titr.direction: ....................................... 16 99 Tree ..........................................................52ff Trigger....................................................... 47 transmission error.................................. U Unit result .................................................... 26 sample........................................... 37, 39 up lim....................................................... 19 U(pol) ....................................................... 17 <USER> .................................................. 34 <USER METH> ....................................... 35 User methods ................................... 35, 129 User name ................................................ 34 delete ................................................... 34 V validate instrument ................................ 99 Validation ................................................ 139 validation: ................................................ 9 Values input ............................................ 7, 8 Variables CXX ........................................... 26 W Warranty.................................................. 140 wrong sample ............................................ 99 T Technical specifications.......................... 123 t(delay) .................................................... 16 temperature ............................................... 17 Text input..................................................... 8 time ........................................................... 11 time counter ............................................... 9 time interval ............................................. 9 time-out PC keyboard .............................. 99 Titration problems.............................................. 24 vessel ................................................. 122 Titration curve changing output .................................. 13 display.................................................. 33 examples.............................................. 32 printing ................................................. 31 Titration modes ......................................... 14 Titration parameters KFT .......................... 15 Titration sequence KFT ............................. 20 150 795 KFT Titrino